Amides-buliding-blocks

Related Products of 21440-97-1, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 21440-97-1 as follows.

Example 6 Preparation of 6-bromo-4,4-dimethyl-benzoxazine-2-one Lithium Salt Similarly, 6-bromo-4,4-dimethyl-benzoxazine-2-one (2.55 g) was reacted with lithium tert-butoxide (10 mL of 1M solution in THF). After evaporation a brownish solid was obtained (3.35 g; quant. yield) that was soluble in dimethyl pyrimidone (DMPU) without heating. 1H NMR (DMSO-d6) did not show a peak corresponding to a N-H group.

According to the analysis of related databases, 21440-97-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Wyeth; US2005/250766; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 16982-21-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 16982-21-1 name is Ethyl 2-amino-2-thioxoacetate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Ethyl thiooxamate (1.0 Kg, 7.52 mol) was added portion-wise to a solution of 2- bromopyruvic acid (1.38 Kg, 8.27 mol) in THF (4 L) over 20 min while the reaction was cooled with water bath. The reaction mixture was stirred for 12 h at room temperature. The reaction mixture was filtered to remove solid. The filtrate was concentrated to dryness to afford crude compound 70-1 (1.8 kg). The crude 70-1 was triturated with EtOAc/hexane/H20 (1 :3 :2, 6 L), filtered, and the solid was further triturated with EtO Ac/hexane (1 :8, 3 L), filtered, and the solid was dissolved in DCM (6 L), dried over anhydrous Na2S04, concentrated to afford compound 70-1 (617 g, 41% yield based on ethyl thiooxamate) as light yellow solid. 1H NMR (400 MHz, CDCI3): d 8.79 (s, 1H), 4.38-4.46 (q, J= 7.2 Hz, 2H), 1.3-1.38 (t, J= 7.2 Hz, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethyl 2-amino-2-thioxoacetate, and friends who are interested can also refer to it.

Reference:
Patent; ARIAGEN, INC.; COLABUONO, Peter; JOHNSON, Graham; MANNING, David Douglas; WOLF, Mark Allan; (312 pag.)WO2019/99977; (2019); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 121496-39-7, name is tert-Butyl benzyl(2-hydroxyethyl)carbamate, A new synthetic method of this compound is introduced below., SDS of cas: 121496-39-7

Under nitrogen atmosphere, to an ice-cooled solution of 4-iodophenol (15.40 g), triphenylphosphine (22.03 g), and tert-butyl benzyl (2-hydroxyethyl) carbamate (21.05 g) in tetrahydrofuran (123 ml) was added diethyl azodicarboxylate (14.58 g) in tetrahydrofuran (31 ml) for 25 minutes, and the mixture was stirred at room temperature for 2 hours. After being concentrated, the mixture was treated with HEXANE/ETHYL acetate (5/1, 180 ml). The precipitate formed was filtered off, the filtrate was concentrated, and the residue was purified by column chromatography (silica gel, hexane/ethyl acetate) to give tert-butyl benzyl [2- (4- iodophenoxy) ethyl] carbamate (7.17 G) as a colorless oil. NMR (CDC13, B) : 1.45 (9H, s), 3.58 (2H, br s), 4.07 (2H, br s), 4.55 (2H, s), 6.62 (2H, d, J=8Hz), 7.10- 7.40 (5H, m), 7.53 (2H, d, J=8HZ) (+) ESI-MS (m/z): 476 (M+Na) +

The synthetic route of 121496-39-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FUJISAWA PHARMACEUTICAL CO., LTD; WO2004/45610; (2004); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 919475-15-3, name is 2-(4-(Benzyloxy)phenyl)-N,N-dimethylacetamide, A new synthetic method of this compound is introduced below., SDS of cas: 919475-15-3

A solution of 2N lithium diisopropylamide (LDA) (48.25 mL, 96.5 mmol) was cooled to -78¡ã C. and diluted with 25 mL of tetrahydrofuran (THF). To this was added dropwise, a solution of 2-(4-Benzyloxy-phenyl)-N,N-dimethyl-acetamide (20 g, 74.3 mmol) in 250 mL of THF. The mixture was warmed to 0¡ã C., then cooled back to -78¡ã C. A solution of 1,4-cyclohexanedione mono-ethylene ketal (14.1 g) in 350 mL of THF was added. The solution was allowed to warm to -20¡ã C. Highthroughput liquid chromatography (HPLC) assay still showed starting material. Another 1 g of ketal was added and the solution was warmed to 0¡ã C. for 2 hour. The reaction was quenched with a mixture of 25 g NH4Cl in 200 mL of water. EtOAc was added and the layers separated. The organic layer was dried with MgSO4, filtered and concentrated. Column chromatography (50percent EtOAc/hexanes) gave 30.3 g, 96percent yield of a solid

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Wyeth; US2007/15828; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 67046-22-4, The chemical industry reduces the impact on the environment during synthesis 67046-22-4, name is 6,7-Dihydro-5H-pyrido[2,3-b]azepin-8(9H)-one, I believe this compound will play a more active role in future production and life.

At -78C, 4.5 mL of 2.0 M lithium diisopropylamide-tetrahydrofuran solution and 300 mg of paraformaldehyde were added to tetrahydrofuran (30 mL) solution of 367 mg of the compound of the above 1, and gradually heated up to room temperature. At room temperature, this was stirred overnight, and then water was added to the reaction liquid and extracted with ethyl acetate. The ethyl acetate layer was dried with anhydrous sodium sulfate, the solvent was evaporated off under reduced pressure, and the residue was separated and purified through partitioning thin-layer chromatography (chloroform/methanol = 10/1) to obtain 111 mg of the entitled compound.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 6,7-Dihydro-5H-pyrido[2,3-b]azepin-8(9H)-one, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BANYU PHARMACEUTICAL CO., LTD.; EP1726590; (2006); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 142733-64-0,Some common heterocyclic compound, 142733-64-0, name is tert-Butyl (cis-3-(hydroxymethyl)cyclobutyl)carbamate, molecular formula is C10H19NO3, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a solution of II-29-1 (200 mg, 1.0 mmol) and Et3N (202 mg, 2.0 mmol) in CH2C12(10 mL) was added MsCl (172 mg, 1.5 mmol) at 0 C. The reaction mixture was stirred at room temperature overnight before water was added to the reaction. The solution mixture was extracted with CH2C123 times. The organic layer was washed with brine and dried over Na2S04. The solution was filtered and concentrated to give II-29-2 as a white solid (250 mg, yield: 90%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route tert-Butyl (cis-3-(hydroxymethyl)cyclobutyl)carbamate, its application will become more common.

Reference:
Patent; KURA ONCOLOGY, INC.; BURROWS, Francis; KESSLER, Linda V.; LI, Liansheng; REN, Pingda; WANG, Yi; WU, Tao; ZHANG, Jingchuan; (355 pag.)WO2018/175746; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 112257-19-9,Some common heterocyclic compound, 112257-19-9, name is tert-Butyl methyl(2-(methylamino)ethyl)carbamate, molecular formula is C9H20N2O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a solution of Compound 79-4a (510 mg, 1.57 mmol) in DCE (5 mL) at 25¡ã C. was added tert-butyl N-methyl-N-[2-(methylamino)ethyl]carbamate (300 mg, 1.59 mmol, 1.01 eq). The mixture was stirred for 1 h, AcOH (52.50 mg, 0.874 mmol, 0.0556 eq) and NaBH(OAc)3 (666.47 mg, 3.14 mmol, 2 eq) were added and the mixture was stirred at RT for 3 hr, then partitioned between saturated aq. NaHCO3 (50 mL) and EtOAc (100 mL). The organic layer was washed with brine (50 mL), dried (Na2SO4), filtered and concentrated under reduced pressure to give the title compound (0.77 g, 1.38 mmol, 88percent yield) as yellow oil. MS (ES+) C26H42F2N4O3, requires: 496, found: 497 [M+H]+.

The synthetic route of 112257-19-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Board of Regents, The University of Texas System; DI FRANCESCO, Maria Emilia; JONES, Philip; MCAFOOS, Timothy Joseph; (166 pag.)US2019/270739; (2019); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 89979-12-4, These common heterocyclic compound, 89979-12-4, name is 5-Chloro-2-(methylsulfonamido)benzoic acid, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: To a solution of 5-chloro-N,6-dimethyl-2-[(1S)-1-(methylamino)propyl] pyrazolo[1,5-a] pyrimidin-7-amine (97 mg,0.361 mmol) and 5-chloro-2-(methylsulfonamido) benzoic acid(99 mg, 0.397 mmol) in N,N-dimethylformamide (1.0 mL)was added trimethylamine (0.25 mL, 1.80 mmol) and1-[bis(dimethylamino) methylene]-1H-1,2,3-triazolo[4,5-b]-pyridinium 3-oxide hexafluorophosphate (0.17 g, 0.433 mmol).After stirring at room temperature for 1 h, the reaction mixturewas purified by reversed-phase preparative HPLC toobtain 5-chloro-N-{(1S)-1-[5-chloro-6-methyl-7-(methylamino)-pyrazolo[1,5-a] pyrimidin-2-yl] propyl}-2-[(methanesulfonyl)-amino]-N-methylbenzamide (0.13 g, 0.904 mmol, 90%) as acolorless powder

The synthetic route of 89979-12-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yamaguchi-Sasaki, Toru; Tamura, Yunoshin; Ogata, Yuya; Kawaguchi, Takanori; Kurosaka, Jun; Sugaya, Yutaka; Iwakiri, Kanako; Busujima, Tsuyoshi; Takahashi, Ryo; Ueda-Yonemoto, Naoko; Tanigawa, Eiji; Abe-Kumasaka, Tomoko; Sugiyama, Hiroyuki; Kanuma, Kosuke; Chemical and Pharmaceutical Bulletin; vol. 68; 4; (2020); p. 345 – 362;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 118684-31-4,Some common heterocyclic compound, 118684-31-4, name is tert-Butyl (3-(hydroxymethyl)phenyl)carbamate, molecular formula is C12H17NO3, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To the solution of 6 (5g, 22.4mmol) , and TEA (12.54mL, 89.6mmol) in DCM (100mL) was added MsCl (3.47mL, 44.8mmol) in DCM (20mL) dropwise over 20 min at -15 under nitrogen atmosphere. The resulting mixture was warmed to 0, and stir for 16h. The reaction mixture was poured into 100mL water, and stir for 5min. Collected the organic phase, concentrated in vacuo, and purified by column chromatography to give desired protuct 7 (1.86g, 27.6%) .

The synthetic route of 118684-31-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FUJIAN HAIXI PHARMACEUTICALS CO., LTD; FENG, Yan; WANG, Ruyong; LI, Junqing; ZHENG, Jianjia; LIAN, Xin; GONG, Xuan; FU, Yueli; KANG, Xinshan; (144 pag.)WO2019/174601; (2019); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 1032350-06-3, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 1032350-06-3, name is tert-Butyl (1-(4-bromophenyl)cyclobutyl)carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

27.75 g (55 mmol) [1 -(4-Bromo-phenyl)-cyclobutyl]-carbamic acid tert-butyl ester,23.76 mmol (93.6 mmol) bis-(pinacolato)diboron, 25 g (255 mmol) potassium acetate and 2.08 g (2.55 mmol) 1 ,1 ‘-bis(diphenylphosphino)ferrocenedichloro- palladium(ll) in 500 mL degassed THF were heated for three hours at reflux. The colour of the reaction mixture turned from dark red to black. Due to an incomplete reaction heating was continued for another two hours. The reaction mixture was poured on water (400 mL) and diluted with ethyl acetate (700mL). After stirring for 30’ the organic phase was separated and the aqueous phase was reextracted twice with ethyl acetate (400 and 200 mL). The combined organic extracts were washed with brine (200 mL) and dried (sodium sulfate). After evaporation of the solvent the residue was purified by chromatography (Biotage) yielding 28.99 g (91 .3%) of the title compound.1 H NMR (400 MHz, d6-DMSO): delta 7.51 -7.67 (m, 3H), 7.38 (d, 2H), 2.22-2.42 (m, 4H), 1 .88-2.02 (m, 1 H), 1 .63-1 .80 (m, 1 H), 1 .00-1 .38 (m, 21 H) ppm.

The synthetic route of tert-Butyl (1-(4-bromophenyl)cyclobutyl)carbamate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; INCE, Stuart; HAEGEBARTH, Andrea; POLITZ, Oliver; NEUHAUS, Roland; BOeMER, Ulf; SCOTT, William; WO2012/7345; (2012); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics