反应 #50476

反应方程式

compound

4- Chloro-2-(2-methoxy-1-methyl-2-oxoethoxy)benzoic acid, methyl ester

sodium hydride

ammonium chloride

ether

→

desired product

收率 44.4%

6-chloro-2-methyl-3(2H)-benzofuranone

收率 44.4%

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   温度was heated
2. 2
   干燥The ether solution was dried over magnesium sulfate
3. 3
   其他evaporated

实验过程

A mixture of the compound of Example 7, Step A, (6.7 g) and sodium hydride (60% in oil, 1.5 g) was heated to reflux in tetrahydrofuran (50 ml). It Was then allowed to cool to room temperature over 1.5 hrs. The cooled mixture was treated with aqueous ammonium chloride solution and ether. The ether solution was dried over magnesium sulfate and then evaporated. The oil was subjected to chromatography on silica gel with hexanes/ethyl acetate (25:1) as the eluent. The desired product (1.99 g) was obtained as a low melting solid. NMR: 7.6 (d, 1H), 7.1 (m 2H), 4.7 (q, 1H), 1.55 (d, 3H).

来源