Amides-buliding-blocks

Reference of 299430-87-8,Some common heterocyclic compound, 299430-87-8, name is (9H-Fluoren-9-yl)methyl (2-(2-hydroxyethoxy)ethyl)carbamate, molecular formula is C19H21NO4, 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.

[000976] To Example 2.62.3 (5.03 g) and triphenylphosphine (4.62 g) in toluene (88 mL) was added di-fert-butyl-azodicarboxylate (4.06 g) and the reaction was stirred for 30 minutes. (9H- Fluoren-9-yl)methyl (2-(2-hydroxyethoxy)ethyl)carbamate was added and the reaction was stirred for an addition 1.5 hours. The reaction was loaded directly onto silica gel and was eluted with 1-50% ethyl acetate/heptanes to provide the title compound

The synthetic route of 299430-87-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBVIE INC.; TAO, Zhi-Fu; DOHERTY, George; WANG, Xilu; SULLIVAN, Gerard M.; SONG, Xiaohong; KUNZER, Aaron R.; WENDT, Michael D.; MARIN, Violeta L.; FREY, Robin R.; CULLEN, Steve C.; WELCH, Dennie S.; SHEN, Xiaoqiang; BENNETT, Nathan B.; HAIGHT, Anthony R.; ACKLER, Scott L.; BOGHAERT, Erwin R.; SOUERS, Andrew J.; JUDD, Andrew S.; (623 pag.)WO2016/94509; (2016); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 5317-89-5, 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. 5317-89-5 name is N-(4-Acetylphenyl)methanesulfonamide, 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.

A mixture of 4′- (Methylsulfonylamino) acetophenone (13-5,5 mmol) and hydroxylamine hydrochloride (0.695 g, 10 mmol) in pyridine (5 mL) was heated at 70 C for 3 h. The reaction mixture was cooled to room temperature, diluted with H20, and extracted with EtOAc several times. The combined organic layers were washed with H20 and brine, dried over MGS04, filtered, and the filtrate was concentrated in vacuo. The residue was purified by flash column chromatography on silica gel using EtOAc: hexanes (1: 1) as eluant to 4′- (Methylsulfonylamino) acetophenone oxime (13-8, LJO-299). 91% yield, white solid, mp = 180 C ‘H NMR (CDC13) 6 7.65 (dd, 2 H, J= 2,6. 6 Hz, ), 7.29 (s, 1 H), 7.20 (dd, 2 H, J= 2, 6. 8 Hz), 6.43 (bs, 1 H), 3.03 (s, 3 H), 2.26 (s, 3 H)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, N-(4-Acetylphenyl)methanesulfonamide, and friends who are interested can also refer to it.

Reference:
Patent; DIGITALBIOTECH CO., LTD.; WO2005/3084; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

111300-06-2, name is tert-Butyl (trans-4-hydroxycyclohexyl)carbamate, belongs to amides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: tert-Butyl (trans-4-hydroxycyclohexyl)carbamate

ferf-Butyl (frans-4-methoxycyclohexyl)carbamate: In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of ferf-butyl (frans-4-hydroxycyclohexyl)carbamate (200 mg, 0.93 mmol) in CH2CI2 (4.5 mL) at rt was treated with powdered molecular sieves 3A, 1 ,8- bis(dimethylamino)naphthalin (498 mg, 2.32 mmol) and trimethyloxomium tetrafluoroborate (289 mg, 1.86 mmol). The reaction mixture was stirred at rt for 2 days. The reaction mixture was filtered, the org. phase was washed with 1 N aq. HCI, brine, dried over MgS04, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (7:3 hept-EA) gave the title compound as off-white solid: TLC: rf (7:3 hept-EA) = 0.22

The synthetic route of 111300-06-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ACTELION PHARMACEUTICALS LTD; CORMINBOEUF, Olivier; CREN, Sylvaine; LEROY, Xavier; POZZI, Davide; WO2015/19325; (2015); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 144-80-9, These common heterocyclic compound, 144-80-9, name is N-((4-Aminophenyl)sulfonyl)acetamide, 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: A solution of NaNO2 (0.4 g, 5.8 mole in 5 mL H2O) was added drop wise to a well cooled stirred solution of 4-aminobenzenesulfonic acid 2 (0.87 g, 0.005 mol), p-aminobenzenesulphonamide 3 (0.86 g, 0.00 5 mol), N-(4-aminophenylsulfonyl) acetamide 4 (1.07 g, 0.005 mol), 1-(4-aminophenylsulfonyl) guanidine 5 (1.07 g,0 .005 mol) and 4-amino-N-(4,6-dimethylpyrimidin-2-yl) benzenesulfonamide 6 (1.4 g, 0.005 mol) in a mixture of concentrated HCl (3 mL) and H2O (3 mL ). The above cooled diazonium solution was added slowly to a well stirred solution of curcumin 1 (1.84 g,0.005 mol) in pyridine (25 mL). The reaction was stirred for 2 h. The formed precipitate was filtered off, dried and crystallized from EtOH/benzene to give the sulpha derivatives 12, 13, 14, 15 and 16, respectively.

Statistics shows that N-((4-Aminophenyl)sulfonyl)acetamide is playing an increasingly important role. we look forward to future research findings about 144-80-9.

Reference:
Article; Gouda, Moustafa A.; Hussein, Belal H.M.; Letters in drug design and discovery; vol. 14; 12; (2017); p. 1425 – 1432;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 614-76-6, These common heterocyclic compound, 614-76-6, name is 2-BroMoacetanilide, 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.

A mixture of aa (2.0 g, 9.34 mmol), tributylvinyl stannane (3.55 mL, 12.15 mmol) and Pd(PPh3)2Cl2 (1.64 g, 2.335 mmol) in toluene was heated at 95 C. under nitrogen after degassing. After 1 hour, the reaction mixture was concentrated and purified by flash chromatography (SiO2, 100% CH2Cl2 to 50% EtOAc/CH2CL2) followed by recrystalization from EtOH/H2O to give bb (732 mg, 49%). HPLC Rt=1.45 min.

Statistics shows that 2-BroMoacetanilide is playing an increasingly important role. we look forward to future research findings about 614-76-6.

Reference:
Patent; Gavai, Ashvinikumar V.; Norris, Derek J.; Han, Wen-Ching; Vite, Gregory D.; Fink, Brian E.; Tokarski, John S.; US2005/192310; (2005); 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. 956434-30-3, name is tert-Butyl 8-chloro-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate, A new synthetic method of this compound is introduced below., Recommanded Product: tert-Butyl 8-chloro-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate

(step 1) To a solution of 3,3-dimethylbutan-2-ol (0.18 mL) in toluene (4 mL) was added sodium hydride (0.14 g), and the resulting mixture was stirred at 70C for 15 min under a nitrogen atmosphere. A mixture of tert-butyl 8-chloro-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate (0.50 g), BINAP (0.033 g), Pd2(dba)3 (0.024 g) and toluene (4 mL) was added, and the resulting mixture was stirred at 100C for 2 hr under an argon atmosphere. The reaction solution was poured into water, and the resulting product was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (solvent gradient; 0?40% ethyl acetate/hexane) to give tert-butyl 8-(1,2,2-trimethylpropoxy)-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate (0.38 g, 62%) as a white powder. 1H-NMR(CDCl3):delta0.95(9H,s), 1.20(3H,d,J=6.4Hz), 1.43(9H,s), 3.80-3.83(2H,m), 4.22(2H,brs), 4.34-4.50(2H,m), 4.91(1H,brs), 6.39(1H,d,J=8.1Hz), 7.30-7.55(1H,m)

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; Takeda Pharmaceutical Company Limited; EP2213675; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 337463-88-4, name is 6-Bromo-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one, 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. SDS of cas: 337463-88-4

(d) 6-((¡ê)-Styryl)-4H-pyrido[3,2-¡ê>][1 ,4]oxazin-3-one; 6-Bromo-4H-pyrido[3,2-b][1 ,4]oxazin-3-one (6.0 g, 26.3 mmole) and trans-2- phenylvinylboronic acid (3.9 g, 26.3 mmole) were dissolved in 1 ,4-dioxane (150 mL) and the solution was degassed with argon. (Ph3P)4Pd (230 mg, 0.2 mmole) was added, followed by a solution of potassium carbonate (6.9 g, 50 mmole) in H2O (20 mL). The reaction was heated at reflux under argon overnight, then was cooled to room temperature and diluted with EtOAc (200 mL). The solution was washed sequentially with H2O and brine, dried (Na2SC>4), and concentrated in vacuo. The solid residue was purified by flash chromatography on silica gel (5-10% EtOAc/CHCl3) to afford a solid (2.5 g, 38%): MS (ES) m/z253.0 (M + H)+.

The synthetic route of 6-Bromo-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2006/81179; (2006); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 88829-82-7, 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. 88829-82-7 name is tert-Butyl (8-aminooctyl)carbamate, 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.

General procedure 2. Starting compound III: S-Methyl N-cyano-N’-4-pyridylisothiourea. Starting compound IV: 8-t-Butoxycarbonylaminooctylamine. Purification: General procedure. 13C NMR (CDCl3) delta: 157.3, 155.5, 149.8, 146.1, 116.4, 114.5, 77.2, 41.7, 29.4, 28.6, 28.6, 28.2, 26.1, 26.0.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, tert-Butyl (8-aminooctyl)carbamate, and friends who are interested can also refer to it.

Reference:
Patent; Leo Pharmaceutical Products, Ltd. A/S; US6346520; (2002); B1;,
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. 24036-52-0, name is 6-Bromo-2H-1,4-benzoxazin-3(4H)-one, A new synthetic method of this compound is introduced below., Recommanded Product: 6-Bromo-2H-1,4-benzoxazin-3(4H)-one

Step II: To a stirred solution of 6-bromo-2H-1,4-benzoxazin-3(4H)-one (10 g, 43.85 mmol) in THF (25 ml) was added 1.0 M borane-tetrahydrofuran complex in THF (153.5 ml, 153.48 mmol) and refluxed for 14 h. The reaction mixture was cooled to room temperature, quenched with methanol (50 ml) and concentrated under reduced pressure. The resulting residue was taken in ethyl acetate (100 ml), washed with aqueous saturated sodium bicarbonate solution (100 ml), water (100 ml), brine (100 ml), dried over sodium sulphate, concentrated and purified by silica gel column chromatography (5% ethyl acetate in hexane) to provide 6-bromo-3,4-dihydro-2H- benzop^oxazine (8.5 g).

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; NOVARTIS AG; BEBERNITZ, Gregory Raymond; BHOSALE, Sandeep Bhausaheb; BHUNIYA, Debnath; HAJARE, Atul Kashinath; MENGAWADE, Tanaji; MUKHOPADHYAY, Partha P.; PALLE, P. Venkata; REDDY, Dumbala Srinivas; WO2010/128152; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 4815-28-5,Some common heterocyclic compound, 4815-28-5, name is 2-Amino-4,5,6,7-tetrahydro-1-benzothiophene-3-carboxamide, molecular formula is C9H12N2OS, 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.

Example 492-(2-(3-(trifluoromethyl)-4,5,6,7-tetrahydroindazole-1-yl)propanamido)-4,5,6,7- tetrahydrobenzorithiophene-3-carboxamide a) 2-(3-chloropropanamido)-4,5,6,7-tetrahydrobenzo[]thiophene-3-carboxamide2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide (250 mg, 1.28 mmol) and triethylamine (0.18 ml_, 1.28 mmol) were stirred in DCM (5 ml_). 3-chloropropionylchloride (162 mg, 1.28 mmol) was added dropwise under a nitrogen atmosphere. Stirring was continued for 2 h. 2 M HCI (20 ml_) was added and the reaction mixture extracted into DCM (3 x 50 ml_), The combined DCM layers were washed with brine, dried over MgSO4, filtered and the solvent removed in vacuo to give the desired product as a yellow solid (290 mg, 1.01 mmol, 79 %).1 H NMR (400MHz, CDCI3): delta 1.86 (m, 4H), 2.72 (m,4H), 2.91 (t,2H), 3.86 (t, 2H), 5.73 (s, 2H), 12.1 (s,1 H).

The synthetic route of 4815-28-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; N.V. ORGANON; WO2008/3452; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics