تفاعل #1260294

معادلة التفاعل

sulfur dioxide

sulfathiazole

hydrochloric acid

sodium nitrite

→

4-chlorosulfonyl-N-(2-thiazolyl)benzenesulfonamide

المذيبات

acetic acid

acetic acid

water

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGby stirring at 5° C. for about 10 minutes
2. 2
   تركيزby saturating 18 ml of acetic acid with sulfur dioxide
3. 3
   workup.ADDITIONadding 830 mg of cupric chloride
4. 4
   workup.ADDITIONdihydrate thereto) was added dropwise to the reaction solution at 0° C.
5. 5
   workup.STIRRINGunder stirring
6. 6
   workup.ADDITIONthe reaction solution was poured into ice-water
7. 7
   ترشيحThe precipitates were collected by filtration
8. 8
   غسيلwashed with water
9. 9
   أخرىdried

الإجراء التجريبي

5.2 g (20.4 mmol) of sulfathiazole was added to a mixed solution of 14 ml of water and 3.4 ml of concentrated hydrochloric acid and the mixture was stirred. To the mixture was added dropwise an aqueous saturated solution of 2.1 g (30.4 mmol) of sodium nitrite at 0° C. or less. Then, 5 ml of acetic acid was added thereto, followed by stirring at 5° C. for about 10 minutes. An acetic acid solution saturated with sulfur dioxide (solution prepared by saturating 18 ml of acetic acid with sulfur dioxide and then adding 830 mg of cupric chloride.dihydrate thereto) was added dropwise to the reaction solution at 0° C. under stirring. After 5 minutes, the reaction solution was poured into ice-water. The precipitates were collected by filtration, washed with water and dried, to give 2.9 g of 4-chlorosulfonyl-N-(2-thiazolyl)benzenesulfonamide. 570 mg (1.68 mmol) of the product was reacted with 200 mg (1.2 mmol) of the compound of Production Example 1a in the same manner as in Production Example 4a and treated, to give 456 mg of the title compound.

المصدر