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[Indazole]

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CAS
247170-27-0
InChI Key
LGDDDQBFEWZCEW-UHFFFAOYSA-N

[mishka]

NMR Spectroscopy - 1

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Nucleus (NMR Spectroscopy) Solvents (NMR Spectroscopy) Frequency (NMR Spectroscopy), MHz Original Text (NMR Spectroscopy) Location Comment (NMR Spectroscopy) Reference
1H
dimethylsulfoxide-d6
300
'H-NMR (300 MHz, DMSO-d6) δ 7.79 (br s, 1H), 7.86- 7.95 (m, 3H), 8.26 (br s, 1 H).
Page/Page column 23
Signals given
Current Patent Assignee: GLENMARK PHARMACEUTICALS - WO2011/132017, 2011, A1

там же
Colour & Other Properties
white
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Получение

Stage #1: 3-fluoro-4-(trifluoromethyl)benzoic acid With oxalyl dichloride; N,N-dimethyl-formamide In dichloromethane at 0 - 20℃; for 2h;
Stage #2: With ammonia In water; acetone at 0 - 20℃; for 2h;

Experimental Procedure
Current Patent Assignee: GLENMARK PHARMACEUTICALS - WO2011/132017, 2011, A1
Location in patent: Page/Page column 23

Full Text

Details

Abstract
2.1
Step 1 ; 3-Fluoro-4-(trifluoromethyl)benzamide: To a stirred solution of 3-fluoro-4- (trifluoromethyl)benzoic acid (2.8 g, 13.46 mmol), dry DMF ( 1 -2 drops) in dry dichloromethane (30 ml) was added oxalyl chloride (1.4 ml, 16.15 mmol) drop wise at 0- 5°C and stirred at room temperature for 2 h. The excess of solvent was evaporated under reduced pressure. The acid chloride was dissolved in dry acetone and was added to aqueous ammonia solution (50 ml) at 0-5°C. Reaction mixture was stirred at room temperature for 2 h and resulting solid was filtered and dried to yield 2.51 g of white solid.'H-NMR (300 MHz, DMSO-d6) δ 7.79 (br s, 1H), 7.86- 7.95 (m, 3H), 8.26 (br s, 1 H).

[Indazole]

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