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
Sodium hydroxide (12 mL, 6M) was added to a solution of ethyl 5-(3-benzenesulfonylpropyl)-1-butyl-1H-pyrazole-3-carboxylate (13.3 g, 35.1 mmol) in 100 mL of ethanol and heated to reflux overnight. The reaction mixture was concentrated under reduced pressure and the residue was diluted with 100 mL of water. The aqueous layer was extracted with several portions of ethyl acetate. The pH of the aqueous layer was adjusted to approximately 2-3 with aqueous hydrochloric acid and was then extracted with several portions of ethyl acetate. The combined organic layers originating from extraction of the aqueous layer were washed with brine, dried over magnesium sulfate, filtered, and concentrated to afford 10.5 g of 5-(3-benzenesulfonylpropyl)-1-butyl-1H-pyrazole-3-carboxylic acid.
WORKUP
后处理
- temperatureheated
- temperatureto reflux overnight
- concentrationThe reaction mixture was concentrated under reduced pressure
- additionthe residue was diluted with 100 mL of water
- extractionThe aqueous layer was extracted with several portions of ethyl acetate
- extractionwas then extracted with several portions of ethyl acetate
- extractionThe combined organic layers originating from extraction of the aqueous layer
- washwere washed with brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated