HRID2380641
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe whole was heated
- temperatureunder reflux for 72 hours
- customThe reaction was terminated
- temperatureby cooling with ice-water
- additionadding saturated ammonium chloride aq solution
- filtrationThen, the organic layer was filtered off
- additionthe solid residue was treated with 10% hydrochloric acid
- extractionextracted with diethyl ether
- dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
- filtrationafter filtration
- concentrationconcentrated