HRID729275

反应详情

EQUATION

反应方程式

HRID 729275 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 2-butyl-4-chloro-5-phenylisothiazol-3(2H)-one 1,1-dioxide (300 mg, 0.90 nmol) and 1-(5-amino-1-benzofuran-2-yl)ethanone (387 mg, 2.21 mmol) in dry MeCN (4.5 mL) was heated in a microwave reactor at 130° C. for 1 h, then at 130° C. for 1 h, then at 140° C. for 1 h and finally at 140° C. for 1.5 h. The mixture was purified using preparative HPLC (Kromasil-column C8, 0.1M NH4OAc/MeCN, gradient) to give the title compound (116 mg, 28%); 1H NMR (400 MHz, CD3CN): δ 7.86 (bs, 1H), 7.34-7.32 (m, 1H), 7.26-7.22 (m, 1H), 7.03-7.15 (m, 7H), 3.76 (t, 2H), 1.78-1.87 (m, 2H) 1.43-1.54 (m, 2H), 1.05 (t, 3H); Mass Spectrum: M−H+ 437

WORKUP

后处理

  1. waitat 140° C. for 1 h
  2. waitfinally at 140° C. for 1.5 h
  3. customThe mixture was purified