反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 1-[[2-(trimethylsilyl)ethoxy]methyl]-1H-imidazole-2-carboxaldehyde (prepared according to procedures described by J. P. Whitten et al., J. Org. Chem., 51 (1986), 1891) (9.95 g, 44.0 mmol) in dry ether (40 ml) was dropped into a suspension of lithium aluminum hydride (0.42 g, 12.0 mmol) in dry ether (40 ml) and stirring was continued for 4 hours at room temperature. Then ice-water was added carefully, and the precipitated aluminum hydroxide was filtered off and washed with ether. The aqueous phase was separated and the organic phase was washed with water, dried over sodium sulfate an evaporated in vacuo to leave an oil (9.0 g) which crystallized spontaneously. Yield: 7.1 g, m.p. 68°-69° C. (from pentane).
WORKUP
后处理
- filtrationthe precipitated aluminum hydroxide was filtered off
- washwashed with ether
- customThe aqueous phase was separated
- washthe organic phase was washed with water
- dry with materialdried over sodium sulfate
- customan evaporated in vacuo