HRID1975670
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
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
A mixture of 9 g of methyl 3-(3-cyclohexenyl)-5-chlorosalicylate and 20 ml trifluoroacetic acid is heated at 70° C. overnight. The cooled reaction mixture is diluted with hexanes, washed three times with water, dried and evaporated to dryness. The residue is purified with flash chromatography using 10% ethyl acetate/hexane to give four fractions. First fraction 2.29 of material (mixture of at least two materials); second fraction 2.29 cis isomer; third fraction 1.69 mixture of cis and trans isomers; and fourth fraction 19 trans isomer.
WORKUP
后处理
- customThe cooled reaction mixture
- washwashed three times with water
- customdried
- customevaporated to dryness
- customThe residue is purified with flash chromatography
- customto give four fractions
- additionFirst fraction 2.29 of material (mixture of at least two materials)
- additionthird fraction 1.69 mixture of cis and trans isomers