Tag: 13999-39-8

13999-39-8, 3-Amino-4,5-dimethylisoxazole is a Isoxazoles compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

STEP07: Synthesis of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethyl-isoxazol-3yl) amide.; The solution of 5-Methyl thiophene-2-sulphonyl chloride (10.5 gm, 0.053 mol) in (15ml) methylene chloride was added to the solution of 3-amino-4, 5-dimethylisoxazole (4 gm, 0.035 mol) and dimethylaminopyridine (500 mg) in pyridine (20 ml) at 0 C. After the completion of the addition the temperature of the reaction mixture was slowly raised to room temperature and stirred for 6 hours. The reaction mixture was then concentrated under vacuum, the residue thus obtained was acidified using IN hydrochloric acid followed by extraction with methylene chloride (100 ml x2). The combined extracts were washed with water and brine solution. Organic layer was then dried over sodium sulphate and concentrated to give 4.0 gm of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethyl- isoxazol-3yl) amide as brown colored solid.; STEP09: Synthesis of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethyl-isoxazol-3yl) amide.; The solution of 5-Methyl thiophene-2-sulphonyl chloride (10.5 gm, 0.053 mol) in (15ml) methylene chloride was added to the solution of 3-amino-4, 5-dimethylisoxazole (4 gm, 0.035 mol) and dimethylaminopyridine (500 mg) in pyridine (20 ml) at 0 C. After the completion of the addition the temperature of the reaction mixture was slowly raised to s room temperature and stirred for 6 hours. The reaction mixture was then concentrated under vacuum, the residue thus obtained was acidified using IN hydrochloric acid followed by extraction with methylene chloride (100 ml x2). The combined extracts were washed with water and brine solution. Organic layer was then dried over sodium sulphate and concentrated to give 4.0 gm of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethyl- o isoxazol-3yl) amide as brown colored solid.; STEP05: Synthesis of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethyl-isoxazol-3yl) amide.; The solution of 5-Methyl thiophene-2-sulphonyl chloride (10.5 gm, 0.053 mol) in (15ml) methylene chloride was added to the solution of 3-amino-4, 5-dimethylisoxazole (4 gm, 0.035 mol) and dimethylaminopyridine (500 mg) in pyridine (20 ml) at 0 C. After the completion of the addition the temperature of the reaction mixture was slowly raised to room temperature and stirred for 6 hours. The reaction mixture was then concentrated under vacuum, the residue thus obtained was acidified using IN hydrochloric acid followed by extraction with methylene chloride (100 ml x2). The combined extracts were washed with water and brine solution. Organic layer was then dried over sodium sulphate and concentrated to give 4.0 gm of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethyl- isoxazol-3yl) amide as brown colored solid.; STEPIl: Synthesis of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethyl-isoxazol-3yl) amide.; The solution of 5-Methyl thiophene-2-sulphonyl chloride (l.Ogm, 0.081mol) in (25ml) methylene chloride was added to the solution of 3-amino-4, 5-dimethylisoxazole (6.2gm, 0.055mol ) and dimethylaminopyridine (500 mg) in pyridine (40 ml) at 0 C. After the completion of the addition the temperature of the reaction mixture was slowly raised to room temperature and stirred it for 6 hours. The reaction mixture was then concentrated under vacuum, the residue thus obtained was acidified using IN hydrochloric acid followed by extraction with methylene chloride (100 ml x2). The combined extracts were washed with water and brine solution. Organic layer was then dried over sodium sulphate and concentrated to give 18 gm of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethyl- isoxazol-3yl) amide as brown colored solid.; STEP05: Synthesis of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethyl-isoxazol-3yl) amide.; The solution of 5-Methyl thiophene-2-sulphonyl chloride (16.0gm, 0.08 lmol) in (25ml) methylene chloride was added to the solution of 3-amino-4, 5-dimethylisoxazole (6.2gm, 0.055mol ) and dimethylaminopyridine (500 mg) in pyridine (40 ml) at 0 C. After the completion of the addition the temperature of the reaction mixture was slowly raised to room temperature and stirred it for 6 hours. The reaction mixture was then concentrated under vacuum, the residue thus obtained was acidified using IN hydrochloric acid followed by extraction with methylene chloride (100 ml x2). The combined extracts were washed with water and brine solution. Organic layer was then dried over sodium sulphate and concentrated to give 18 gm of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethyl- isoxazol-3yl) amide as brown colored solid.; STEP05: Synthesis of 5-methyl-thiophene-2-sulphonic acid (4, 5-dimethgammal-isoxazol-3yl) amide.; The solution of 5-Methyl thiophene-2-sulphonyl chloride (l.Ogm, 0.08 lmol) in (25ml) methylene chloride was added to the solution of 3-amino-4, 5-dimethylisoxazole (6.2gm, 0.055mol ) and dimethylaminopyridine (500 mg) in pyridine (40 ml) at 0 C. After the completion of the addition the temperature of the reaction mi…

13999-39-8, The synthetic route of 13999-39-8 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; TORRENT PHARMACEUTICALS LTD; WO2007/100295; (2007); A1;,
Isoxazole – Wikipedia
Isoxazole | C3H3NO – PubChem

13999-39-8, 3-Amino-4,5-dimethylisoxazole is a Isoxazoles compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A 10-mL RBF was charged with (P)-perfluorophenyl perfluorophenyl 1-(4-bromo-5-fluoro-2-methoxyphenyl)-2-oxo-1,2-dihydroquinoline-6-sulfonate (58 mg, 0.098 mmol) and 4,5-dimethylisoxazol-3-amine (16.4 mg, 0.146 mmol) then purged with nitrogen. Tetrahydrofuran (732 muL) and dimethyl sulfoxide (244 muL) were introduced, and the resultant brown solution cooled to 0 C. A solution of lithium bis(trimethylsilyl)amide in tetrahydrofuran (1.0 M, 215 muL, 0.215 mmol) was added dropwise via syringe to the stirred reaction mixture over 3 min. After 15 min, 1.0 N HCl (5 mL) was introduced and the resultant reaction mixture was allowed to warm to ambient temperature. The mixture was diluted with and EtOAc (10 mL) and the layers were separated, and the aqueous layer was further extracted with EtOAc (3*10 mL). The combined organic layers were then washed with brine (20 mL), dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to furnish a yellow oil, which was dissolved in DMSO (2 mL) filtered through a 0.2 micron filter and purified by reverse-phase HPLC (Waters XBridge Prep Shield RP18 10 mum OBD 19*100 mm) gradient, 20 to 75% MeCN in water (containing 0.1% trifluoroacetic acid as an additive), flow rate 40 mL/min to afford (P)-1-(4-bromo-5-fluoro-2-methoxyphenyl)-N-(4,5-dimethyl-3-isoxazolyl)-2-oxo-1,2-dihydro-6-quinolinesulfonamide (29.0 mg, 0.056 mmol, 56.9% yield) as a white amorphous solid. 1 H NMR (500 MHz, DMSO-d6) delta ppm 10.79 (br. s., 1 H) 8.32 (d, J=2.01 Hz, 1 H) 8.23 (d, J=9.67 Hz, 1 H) 7.85 (dd, J=8.99, 2.04 Hz, 1 H) 7.67 (d, J=6.23 Hz, 1 H) 7.62 (d, J=8.56 Hz, 1 H) 6.86 (d, J=8.95 Hz, 1 H) 6.79 (d, J=9.67 Hz, 1 H) 3.70 (s, 3 H) 2.21 (s, 3 H) 1.80 (s, 3 H). m/z (ESI) 522.0 (M+H)+., 13999-39-8

13999-39-8 3-Amino-4,5-dimethylisoxazole 84148, aIsoxazoles compound, is more and more widely used in various.

Reference£º
Patent; Amgen Inc.; Weiss, Matthew; Boezio, Alessandro; Boezio, Christiane; Butler, John R.; Chu-Moyer, Margaret Yuhua; Dimauro, Erin F.; Dineen, Thomas; Graceffa, Russell; Guzman-Perez, Angel; Huang, Hongbing; Kreiman, Charles; La, Daniel; Marx, Isaac E.; Milgrim, Benjamin Charles; Nguyen, Hanh Nho; Peterson, Emily; Romero, Karina; Sparling, Brian; US9212182; (2015); B2;,
Isoxazole – Wikipedia
Isoxazole | C3H3NO – PubChem

13999-39-8, 3-Amino-4,5-dimethylisoxazole is a Isoxazoles compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A. 2-Bromo-N-(4,5-dimethyl-3-isoxazolyl)benzenesulfonamide To 4,5-dimethyl-3-isoxazolamine (1.62 g, 13.00 mmol, prepared as described in T. Konoike et al., Tetrahedron Letters, 37, 3339 (1996)) and 4-dimethylaminopyridine (159 mg, 1.3 mmol) in 6.5 ml pyridine at 0 C., 2-bromobenzenesulphonyl chloride (3.65 g, 14.3 mmol) was added in portions over 10 minutes. After stirring at room temperature overnight, the mixture was added dropwise to 40 ml 6N HCl at 0 C. The mixture was extracted with 3*50 ml EtOAc. The combined organic extracts were washed with 30 ml each of 1N HCl and brine and dried and concentrated. The residue was dissolved in 160 ml MeOH and 160 ml 3% aqueous NaHCO3 solution was added and the mixture was concentrated in vacuo to remove most of the MeOH. The solid was filtered off and the aqueous filtrate was acidified to pH 2 with solid NaHSO4, and extracted with 3*100 ml of EtOAc. The extracts were washed with brine, dried and concentrated to give the title compound of this step (3.0 g, 70%). Rf=0.57, silica gel, 1:1 hexane/EtOAc.

13999-39-8 3-Amino-4,5-dimethylisoxazole 84148, aIsoxazoles compound, is more and more widely used in various.

Reference£º
Patent; Bristol-Myers Squibb Company; US5780473; (1998); A;,
Isoxazole – Wikipedia
Isoxazole | C3H3NO – PubChem