HRID2377631

反应详情

EQUATION

反应方程式

HRID 2377631 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of cyclohexanecarboxaldehyde (10.8 mL, 89.15 mmol) in DCM (500 mL) cooled to 0° C. was added potassium tert-butoxide (13.0 g, 115.9 mmol) and methyl iodide (16.65 mL, 267.5 mmol). After 30 min at this temperature, the mixture was warmed to RT and stirring was continued for an additional 5 h. The reaction was then poured into brine and extracted with DCM. The organic layer was dried over MgSO4 and the solvent was then removed carefully in vacuo to yield 9.4 g (83%) of crude 1-methylcyclohexanecarboxaldehyde which was ˜80% pure and was used directly in the next reaction.

WORKUP

后处理

  1. waitwas continued for an additional 5 h
  2. extractionextracted with DCM
  3. dry with materialThe organic layer was dried over MgSO4
  4. customthe solvent was then removed carefully in vacuo