HRID337602
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
To a suspension of {3-[2-(methyloxy)ethyl]-1-naphthalenyl}methanol (1 eq.) from the previous step and sodium bicarbonate (1.1 eq.) in dichloromethane (0.1 M) was added DMP (1.1 eq.) at 0° C. The resulting mixture was stirred at RT for 2 h before it was quenched with sat. aq. NaHSO3 and then extracted with Et2O. The combined organic extracts were washed further with 1 N aq. NaOH, water and brine, dried over Na2SO4, filtered and the filtrate concentrated in vacuo. Purification of the crude product thus obtained by way of flash chromatography (SiO2, 19:1 (v/v) Hex:EtOAc 1:1 (v/v) Hex:EtOAc) afforded the title compound as a colorless oil.
WORKUP
后处理
- additionwas added DMP (1.1 eq.) at 0° C
- customwas quenched with sat. aq. NaHSO3
- extractionextracted with Et2O
- washThe combined organic extracts were washed further with 1 N aq. NaOH, water and brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationthe filtrate concentrated in vacuo
- customPurification of the crude product
- customthus obtained by way of flash chromatography (SiO2, 19:1 (v/v) Hex:EtOAc 1:1 (v/v) Hex:EtOAc)