Cyclopropanesulfonamide, 1-methyl- (9CI) synthesis
- Product Name:Cyclopropanesulfonamide, 1-methyl- (9CI)
- CAS Number:669008-26-8
- Molecular formula:C4H9NO2S
- Molecular Weight:135.18
923032-55-7
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669008-26-8
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Yield: 77.9%
Reaction Conditions:
with ammonia in diethyl ether at -78 - 25; for 16.5 h;
Steps:
Synthesis of 1-Methylcyclopropane-1-sulfonamide (Int-50)
To a solution of potassium 1-methylcyclopropane-1-sulfonate (4.44 g, 25.5 mmol) in THF (50 mL) at 0° C. was added POCl3 (11.7 g, 76.5 mmol) with stirring, maintaining the same temperature for 30 min. DIPEA (9.8 g, 76.5 mmol) was added to above mixture and continued stirring at 25° C. for 2 h. Reaction mixture was quenched with ice cold water, extracted into diethyl ether (3×100 mL), dried over anhydrous sodium sulphate to afford 1-methylcyclopropane-1-sulfonylchloride in diethyl ether. The above dried ethereal solution of 1-methylcyclopropane-1-sulfonylchloride was cooled to -78° C. and purged in with NH3 gas for 30 min. and slowly allowed the reaction mixture to warm to 25° C. with stirring for 16 h. Reaction mixture was filtered through celite bed and the filtrate was concentrated under reduced pressure and the crude thus obtained was washed with n-pentane to afford 1-methylcyclopropane-1-sulfonamide (Int-50) (2.68 g, 77.9% yield) as pale brown solid. 1H NMR (300 MHz, DMSO-d6) δ 6.7 (2H, s), 1.4 (3H, s), 1.1-1.0 (2H, m) 0.7-0.6 (2H, m) ppm.
References:
Dr. Reddy's Laboratories Ltd.;Sasmal, Pradip Kumar;Ahmed, Shahadat;Tehim, Ashok;Paradkar, Vidyadhar US2015/368238, 2015, A1 Location in patent:Paragraph 0638; 0639
849022-29-3
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669008-26-8
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669008-25-7
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669008-26-8
151 suppliers
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