HRID240714
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
4-Piperidineethanol (2 g, 15.5 mmol) and N,N-diisopropylethylamine (3.00 g, 4.06 ml, 23.2 mmol) were combined with dichloromethane (50 mL) to give a colorless solution. t-Butyldimethylchlorosilane (2.8 g, 18.6 mmol) in dichloromethane (30 mL) was added to this solution during 15 min at 0° C. The reaction mixture was stirred for 2.5 h at 0° C. and afterwards for 21 h at room temperature. Subsequently the reaction mixture was concentrated in vacuo and the residue was crystallized from ethyl acetate and n-heptane (100 ml, 1:1) to give the title compound (3.45 g, 80%) as light yellow solid; GC-MS (EI) 243.0 (M)+.
WORKUP
后处理
- customto give a colorless solution
- concentrationSubsequently the reaction mixture was concentrated in vacuo
- customthe residue was crystallized from ethyl acetate and n-heptane (100 ml, 1:1)