Chlorosulfonic acid → 4-(Chlorosulfonyl)-1,3-dimethyl-1H-pyrazole-5-carboxylic acid

반응식

[CH3:1][N:2]1[C:6]([C:7]([O:9]CC)=[O:8])=[CH:5][C:4]([CH3:12])=[N:3]1.[Cl:13][S:14](O)(=[O:16])=[O:15]>>[CH3:1][N:2]1[C:6]([C:7]([OH:9])=[O:8])=[C:5]([S:14]([Cl:13])(=[O:16])=[O:15])[C:4]([CH3:12])=[N:3]1

참가 물질

반응물 2

HCID 24638Chlorosulfonic acid

HCID 1385761,3-Dimethyl-5-ethoxycarbonylpyrazole

생성물 1

HCID 221675814-(Chlorosulfonyl)-1,3-dimethyl-1H-pyrazole-5-carboxylic acid

반응 조건

온도: 5 °C

실험 절차

Into 200 ml of chlorosulfonic acid, there was added dropwise 50.4 g (0.3 mol) of Ethyl 1,3-dimethyl-5-pyrazole carboxylate under cooling at 5° C. or lower. After heating at 120° C. under stirring for 10 hours, the reaction mixture was poured into ice-water and extracted with ether. After washing with water and drying, evaporation of the solvent gave 49 g of crude 1,3-dimethyl-4-chlorosulfonyl-5-pyrazole carboxylic acid as a solid.

후처리

temperatureAfter heating at 120° C.
extractionextracted with ether
washAfter washing with water
customdrying
customevaporation of the solvent

출처 및 근거

ORD 기록: ord-4bbb62bdeac14d3bb8271c2fd550e715
출처 데이터셋: uspto-grants-1990_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04954164

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