HRID236521

反应详情

EQUATION

反应方程式

HRID 236521 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 10.0 g of 2,3-dichlorobenzenesulfonyl isocyanate in 200 mL of dry tetrahydrofuran was cooled to 0° C. and treated with 5.0 mL of anhydrous liquid ammonia, added in a dropwise manner at a rate that maintained the temperature between 0° and 10° C. The resultant white mixture was allowed to warm to room temperature and was stirred overnight. The precipitate was collected by filtration, dissolved in 250 mL of water, and acidified with concentrated hydrochloric acid to yield a white solid. Filtration and air drying gave 7.0 g of the title compound, m.p. 197°-200° C.; NMR (DMSO-d6): δ6.0-6.8 (br s, 2H), 7.6 (t, 1H), 7.8-8.1 (m, 2H), 11.1 (br s, 1H); IR (nujol): 1690 cm-1.

WORKUP

后处理

  1. additionadded in a dropwise manner at a rate that
  2. temperaturemaintained the temperature between 0° and 10° C
  3. filtrationThe precipitate was collected by filtration
  4. dissolutiondissolved in 250 mL of water
  5. customto yield a white solid
  6. filtrationFiltration and air
  7. customdrying