HRID337602

反应详情

EQUATION

反应方程式

HRID 337602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added DMP (1.1 eq.) at 0° C
  2. customwas quenched with sat. aq. NaHSO3
  3. extractionextracted with Et2O
  4. washThe combined organic extracts were washed further with 1 N aq. NaOH, water and brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationthe filtrate concentrated in vacuo
  8. customPurification of the crude product
  9. customthus obtained by way of flash chromatography (SiO2, 19:1 (v/v) Hex:EtOAc 1:1 (v/v) Hex:EtOAc)