反应 #476754

反应方程式

2-iodoaniline

2-methoxy-thioacetamide

calcium oxide

→

title compound

收率 61.2%

2-methoxymethyl-benzothiazole

收率 61.2%

溶剂

DMF

反应条件

后处理

1. 1
   其他The resulting mixture was purified by column chromatography (10 to 20% ethyl acetate:hexanes)

实验过程

A mixture of 2-iodoaniline (5 g, 22.8 mmol), 2-methoxy-thioacetamide (2.4 g, 22.8 mmol), calcium oxide (1.28 g, 22.8 mmol), tris(dibenzylideneacetone)dipalladium-chloroform adduct (104 mg, 0.114 mmol), diphenylphosphinoferrocine (253 mg, 0.456 mmol) and DMF (23 mL) was stirred at 60° C. for 2 h under nitrogen. The resulting mixture was purified by column chromatography (10 to 20% ethyl acetate:hexanes) to afford 2.5 g (61%) of the title compound. 1H NMR (300 MHz, CDCl3): δ 8.01-7.9 (m, 1H), 7.98-7.89 (m, 1H), 7.50-7.45 (m, 1H), 7.41-7.38 (m, 1H), 4.86 (s, 2H), 3.54 (s, 3H).

来源