HRID66988
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
A mixture of 1.26 g. (10.0 mmoles) of 1-octyn-3-ol, 4.85 g. (15.0 mmoles) of triphenylmethyl bromide, and 50 ml. of dry pyridine is heated at 95° C. for 60 minutes with occasional swirling. The solution is cooled, treated with water, and extracted with ether. The extract is washed successively with water and saturated sodium chloride solution, dried over magnesium sulfate, and concentrated. The crude product is purified by chromatography on Florisil and recrystallization from petroleum ether to give white crystals, m.p. 65°-66.5°, ν max. (KBr) 3280 (acetylenic hydrogen), 1605, 1030, and 702 cm-1 (triphenylmethoxy group).
WORKUP
后处理
- additionA mixture of 1.26 g
- temperatureThe solution is cooled
- extractionextracted with ether
- washThe extract is washed successively with water and saturated sodium chloride solution
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customThe crude product is purified by chromatography on Florisil and recrystallization from petroleum ether
- customto give white crystals, m.p. 65°-66.5°, ν max