反应详情
EQUATION
反应方程式
REACTANTS
反应物
Imidazole
C3H4N2
2,4-Dichloro-1-(chloromethyl)benzene
C7H5Cl3
4-Hydroxyacetophenone
C8H8O2
Thionyl chloride
Cl2OS
Sodium hydride
HNa
2 次
Perchlorate
ClO4-
1-{4-[(2,4-Dichlorophenyl)methoxy]phenyl}ethan-1-ol
C15H14Cl2O2
Sodium borohydride (Na(BH4))
H4BNa
未命名化合物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
136 g. of 4-hydroxyacetophenone is etherified in 500 ml. of dimethylformamide with 30 g. of sodium hydride oil suspension (80%) and 195 g. of 2,4-dichlorobenzyl chloride analogously to Example 16. The thus-obtained 4-(2,4-dichlorobenzyloxy)-acetophenone (290 g., m.p. 89°-90° ) is reduced in 1 liter of ethanol/dioxane (2 : 1) with 50 g. of sodium borohydride analogously to Example 26, and worked up. Of the thusobtained 4-(2,4-dichlorobenzyloxy)-α-methylbenzyl alcohol (m.p. 61°-64°), 1.7 g. is stirred with 5 ml. of thionyl chloride for 1 hour at room temperature. The product remaining after a careful evaporation of the thionyl chloride is reacted according to Example 15 with a solution of sodium imidazole, prepared from 360 mg. of imidazole and 160 mg. of sodium hydride, and converted into the perchlorate as described in Example 26. Yield: 940 mg.; m.p. 103°-106° (methylene chloride/ether).
WORKUP
后处理
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- customprepared from 360 mg