HRID453349
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
The 2-cyanomethyl-(2,3 dihydrobenzo[1,4]dioxine) was dissolved in THF (50 mL) and 1M BH3 in THF (80 mL, 80 mmol) was added and the reaction mixture refluxed for 5 h, then stirred at ambient temperature for 16 h. With ice bath cooling, 2N HCl was added until pH=1.0 was achieved. The reaction mixture was then stirred for 1 h at room temperature and evaporated in vacuo to yield an oil. The oil was partitioned between 3N NaOH and diethyl ether, and the diethyl ether solution was washed with brine, dried (Na2SO4) and evaporated in vacuo to yield crude 2-(2,3 dihydrobenzo[1,4]dioxin-2-yl)ethylamine.
WORKUP
后处理
- temperaturethe reaction mixture refluxed for 5 h
- temperatureWith ice bath cooling
- stirringThe reaction mixture was then stirred for 1 h at room temperature
- customevaporated in vacuo
- customto yield an oil
- customThe oil was partitioned between 3N NaOH and diethyl ether
- washthe diethyl ether solution was washed with brine
- dry with materialdried (Na2SO4)
- customevaporated in vacuo