HRID496166

反应详情

EQUATION

反应方程式

HRID 496166 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cold (0° C. mixture of 100 g (0.891 mole) of cyclohexanecarboxaldehyde, 76.5 g of 37% of formaldehyde in 225 ml of mnethanol was added dropwise 90 ml of 1 N Sodium hydroxide in 1 h. The reaction mixture was stirred at room temperature over 48 then was evaporated to remove methanol. The reaction mixture was diluted with water and extracted with methylene chloride. The organic layer was washed with water, brine, and dried over sodium sulfate and concentrated under vacuum to give 75 g (59.7%) of thick oil. Proton NMR and mass spectra were consistent with the product.

WORKUP

后处理

  1. customthen was evaporated
  2. customto remove methanol
  3. additionThe reaction mixture was diluted with water
  4. extractionextracted with methylene chloride
  5. washThe organic layer was washed with water, brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under vacuum