HRID1066129

反应详情

EQUATION

反应方程式

HRID 1066129 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 2-amino-4-fluorobenzenesulfonamide (1.9 g, 10 mmol) and isopropyl isothiocyanate (6.4 ml, 60 mmol) was heated at 140° C. for 2.5 h. The mixture was cooled to room temperature and stirred with 50 ml of ethyl acetate for 20 min. The precipitate was isolated by filtration and washed with ethyl acetate to give 355 mg (14%) of the title compound; m.p. 266-269° C.; 1H-NMR (DMSO-d6): δ 1.18 (d, 6H, CH(CH3)2), 3.91 (m, 1H, CH(CH3)2), 7.00-7.13 (m, 2H, ArH), 7.16 (br.s, 1H, NH), 7.73 (dd, 1H, ArH), 10.4 (br.s, 1H, NH); MS: m/e 257 (M+, 25%); (C10H12N3F1O2S1) calc. C, 46.68; H, 4.70; N, 16.33; found C, 46.84; H, 4.88; N, 16.13.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. customThe precipitate was isolated by filtration
  3. washwashed with ethyl acetate