HRID1088379
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 stirred mixture of 324 parts of 2-(2,4-dichloro-phenoxy)-1-propanol and 700 parts of N,N-diethylethanamine were added dropwise at room temperature 335 parts of methanesulfonyl chloride (exothermic reaction: the temperature roses to reflux temperature). While cooling in a water-bath, stirring was continued for 30 minutes at room temperature. The reaction mixture was poured onto water and the product was extracted with 2,2'-oxybispropane. The extract was dried, filtered and evaporated. The residue was distilled by vacuum distillation, yielding 300 parts of 2-(2,4-dichlorophenoxy)-1-propanol methanesulfonate (ester); bp. 130° C. at 2×10-4 mm. pressure (intermediate 101).
WORKUP
后处理
- customexothermic reaction
- temperaturethe temperature roses to reflux temperature)
- temperatureWhile cooling in a water-bath
- additionThe reaction mixture was poured onto water
- extractionthe product was extracted with 2,2'-oxybispropane
- customThe extract was dried
- filtrationfiltered
- customevaporated
- distillationThe residue was distilled by vacuum distillation