HRID1066130

反应详情

EQUATION

反应方程式

HRID 1066130 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 (1.71 g, 9 mmol) and cyclopentyl isothiocyanate (4.6 ml, 36 mmol) was heated at 140° C. for 4 h. The mixture was cooled to room temperature and stirred with 50 ml of ethyl acetate. The precipitate was isolated by filtration and recrystallised from ethanol to give 591 mg (23%) of the title compound; m.p. 295-298° C.; 1H-NMR (DMSO-d6): δ 1.37-2.02 (m, 8H, cyclopentyl), 4.05 (sext, 1H, CH), 6.97-715 (m, 2H, ArH), 7.32 (br.s, 1H, NH), 7.72 (dd, 1H, ArH), 10.35 (br.s, 1H, NH; MS: m/e 283 (M+, 21%); (C12H14N3F1O2S1) calc. C, 50.87; H, 4.98; N, 14.83; found C, 50.75; H, 5.12; N, 14.93.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. customThe precipitate was isolated by filtration
  3. customrecrystallised from ethanol