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ChemicalBook CAS DataBase List 4-ISOTHIOCYANATO-N-METHYLBENZENESULFONAMIDE

4-ISOTHIOCYANATO-N-METHYLBENZENESULFONAMIDE synthesis

2synthesis methods
-

Yield:223785-90-8 87%

Reaction Conditions:

with calcium carbonate in dichloromethane;water at 0 - 20; under 760.051 Torr;Inert atmosphere;

Steps:

22 4-isothiocyanato-N-methylbenzenesulfonamide

To a suspension of calcium carbonate (1.34 g, 13.4 mmol, Eq: 2.5) and thiophosgene (679 mg, 453 μ, 5.91 mmol, Eq: 1.1) in dichloromethane (13.2 g, 10.0 ml, 155 mmol, Eq: 28.9)/water (10.0 g, 10.0 ml, 555 mmol, Eq: 103) at 0, was added 4-amino-N- methylbenzenesulfonamide (1 g, 5.37 mmol, Eq: 1.00). The reaction was gradually warmed to room temperature. Added IN HCl slowly. Separated organic layer and dried over sodium sulfate to give 1.064 g (87%) of desired product as a white solid.

References:

WO2014/6066,2014,A1 Location in patent:Paragraph 0202