HRID2380641

反应详情

EQUATION

反应方程式

HRID 2380641 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The resulting THF solution of 1-naphthylmagnesium bromide was cooled to room temperature. Then, a THF (200 ml) solution of (-)-camphor (50 g, 0.328 mol) was added thereto, and the whole was heated under reflux for 72 hours. The reaction was terminated by cooling with ice-water and adding saturated ammonium chloride aq solution. Then, the organic layer was filtered off, and the solid residue was treated with 10% hydrochloric acid and extracted with diethyl ether. The combined organic layer was dried over anhydrous magnesium sulfate and, after filtration, concentrated to give 121 g of a crude (1S)-2-(1-naphthyl)-1,7,7-trimethylbicyclo [2.2.1]-heptan-2-ol as an oil.

WORKUP

后处理

  1. temperaturethe whole was heated
  2. temperatureunder reflux for 72 hours
  3. customThe reaction was terminated
  4. temperatureby cooling with ice-water
  5. additionadding saturated ammonium chloride aq solution
  6. filtrationThen, the organic layer was filtered off
  7. additionthe solid residue was treated with 10% hydrochloric acid
  8. extractionextracted with diethyl ether
  9. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  10. filtrationafter filtration
  11. concentrationconcentrated