HRID1195917

反应详情

EQUATION

反应方程式

HRID 1195917 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 3-carbomethoxy-2,5-dimethylfuran (2.5 g, 16.2 mmol) in methylene chloride (distilled from CaH) at -20° C., under N2, was added 2.5 eq of DIBAL (1M in CH2Cl2). After 1 h, the dry ice/acetonitrile bath was removed and 60 mL of 10% HCl was added dropwise. The organic layer was separated, dried over MgSO4, and evaporated. The residue was chromatographed (silica gel, 60% ether/hexane) to yield 1.3 g of 2,5-dimethyl-3- hydroxymethylfuran.

WORKUP

后处理

  1. customthe dry ice/acetonitrile bath was removed
  2. addition60 mL of 10% HCl was added dropwise
  3. customThe organic layer was separated
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. customThe residue was chromatographed (silica gel, 60% ether/hexane)