HRID1090616
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
Borane-methyl sulphide (2.15g, 2.7ml, 4 equivs.) was added dropwise, under nitrogen, to a stirred solution of N-[1,1-dimethylethyl]-3-chloro-α-hydroxybenzene acetamide (1.71g) in dry tetrahydrofuran. The resulting solution was stirred and heated under reflux for 2h., cooled, and treated with methanol (1ml). The reaction mixture was heated under reflux for 1 h., cooled, treated with methanolic hydrogen chloride, and the solvent evaporated to give 3-chloro-α-[[[1,1-dimethylethyl]amino]methyl]benzenemethanol hydrochloride salt, 1.5g, m.p. 165-175° C.
WORKUP
后处理
- temperatureheated
- temperatureunder reflux for 2h.
- temperaturecooled
- temperatureThe reaction mixture was heated
- temperatureunder reflux for 1 h.
- temperaturecooled
- customthe solvent evaporated