반응 #75897

반응 방정식

hydrochloric acid

2-ethyl-5-methyl-2H-pyrazol-3-ol

calcium hydroxide

benzoyl chloride

→

(1-ethyl-5-hydroxy-3-methyl-1H-pyrazol-4-yl)-phenyl-methanone

용매

water

1,4-dioxane

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred at 110° C. for 2 h
2. 2
   workup.STIRRINGThe mixture was stirred at room temperature for 16 h
3. 3
   추출extracted three times with 60 ml of ethyl acetate
4. 4
   건조The combined extracts were dried over magnesium sulphate
5. 5
   여과filtered
6. 6
   기타evaporated

실험 절차

A suspension of 1.4 g of 2-ethyl-5-methyl-2H-pyrazol-3-ol, 1.6 g of calcium hydroxide and 1.3 ml of benzoyl chloride in 70 ml of 1,4-dioxane was stirred at 110° C. for 3.5 h. 1 ml of water was added and the mixture was stirred at 110° C. for 2 h. 25 ml of 2N hydrochloric acid was added. The mixture was stirred at room temperature for 16 h and extracted three times with 60 ml of ethyl acetate. The combined extracts were dried over magnesium sulphate, filtered and evaporated to give 3.1 g of (1-ethyl-5-hydroxy-3-methyl-1H-pyrazol-4-yl)-phenyl-methanone as a yellow oil which was used without further purification. Mass spectrum (ES) m/z 231 [M+H]+, 272 [M+H+CH3CN]+.

출처