HRID1798804
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
To a solution of sodium t-butoxide (317 mg, 3.3 mmol) in 15 mL EtOH at 0° C. was slowly added 4-methoxybenzenethiol (420 mg, 3 mmol). After completion of addition, the reaction was stirred at RT for 1 hour before cooling down to 0° C. Bromocyclopropane (417 mg, 3.45 mmol) was added slowly, and the mixture was brought to reflux for one hour, cooled and concentrated. Water (1 mL) was added and the mixture was extract with ethyl acetate. The organic phases were dried and purified by column chromatography eluting with 20% ethyl acetate/hexanes to give the desired product.
WORKUP
后处理
- customat 0° C.
- additionAfter completion of addition
- temperaturebefore cooling down to 0° C
- temperatureto reflux for one hour
- temperaturecooled
- concentrationconcentrated
- additionWater (1 mL) was added
- extractionthe mixture was extract with ethyl acetate
- customThe organic phases were dried
- custompurified by column chromatography
- washeluting with 20% ethyl acetate/hexanes