反应 #366641

反应方程式

diisobutylaluminum hydride toluene

methyl 2-(2,5-dimethylphenoxymethyl)-α-methoxyiminophenylacetate

dichloromethane

→

2-(2,5-dimethylphenoxymethyl)-α-methoxyiminophenylacetaldehyde

溶剂

Methanol

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 1 hour
2. 2
   其他The precipitated insoluble materials were removed
3. 3
   浓缩the mixture was concentrated under reduced pressure
4. 4
   其他The residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to 2-(2,5-dimethylphenoxymethyl)-α-methoxyiminophenylacetaldehyde (0.54 g, 36.3%) as a colorless oil

实验过程

1M diisobutylaluminum hydride/toluene solution (5.5 ml, 5.5 mmol) was added dropwise to a mixture of methyl 2-(2,5-dimethylphenoxymethyl)-α-methoxyiminophenylacetate (1.64 g, 5 mmol) and dichloromethane (15 ml) at −70° C. over 0.5 hours, and then the mixture was stirred at −70° C. to room temperature for 3 hours. Methanol (3 ml) was added to the reaction mixture, and the mixture was stirred at room temperature for 1 hour. The precipitated insoluble materials were removed, and the mixture was concentrated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to 2-(2,5-dimethylphenoxymethyl)-α-methoxyiminophenylacetaldehyde (0.54 g, 36.3%) as a colorless oil.

来源