HRID523343

反应详情

EQUATION

反应方程式

HRID 523343 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (±)-1-(3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydro-2-naphthalenyl)-1-ethanone (10.00 g, 38.7 mmol) in ether (65 ml) was added dropwise during 1 h to a suspension of LiAlH4 (1.48 g, 39.0 mmol) in ether (70 ml) at 0° C. The reaction mixture was left warming up to room temperature and then heated to reflux for 1 day. After cooling to 0° C. more LiAlH4 (0.76 g, 19.5 mmol) was added. After refluxing for another 3 days, the mixture was cooled to 0° C. and water was added dropwise. Extraction of the organic phase with water, drying over Na2SO4 and concentrating gave 10.19 g (99%) of the product.

WORKUP

后处理

  1. waitThe reaction mixture was left
  2. temperatureheated
  3. temperatureto reflux for 1 day
  4. additionwas added
  5. temperatureAfter refluxing for another 3 days
  6. temperaturethe mixture was cooled to 0° C.
  7. extractionExtraction of the organic phase with water
  8. dry with materialdrying over Na2SO4
  9. concentrationconcentrating