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Methanesulfonyl chloride → HCID 15077739, 화합물

HRID 2380283
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HRID 2380283 반응식
[OH:1][CH2:2][CH2:3][N:4]1[C:8]([NH2:9])=[C:7]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:6]=[N:5]1.[CH3:15][S:16](Cl)(=[O:18])=[O:17]>C(Cl)Cl.C(N(CC)CC)C>[CH3:15][S:16]([O:1][CH2:2][CH2:3][N:4]1[C:8]([NH2:9])=[C:7]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:6]=[N:5]1)(=[O:18])=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 429881Ethyl 5-amino-1-(2-hydroxyethyl)-1H-pyrazole-4-carboxylate

생성물 1

HCID 15077739HCID 15077739, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

To a solution of 1-(2-hydroxyethyl)-4-ethoxycarbonyl-5-aminopyrazole (200 g) in a mixture of methylene chloride (2 l) and triethylamine (210 ml) was added dropwise methanesulfonyl chloride (85.5 ml) under ice-cooling. The mixture was stirred for 1 hour at 3°-5° C. The reaction mixture was poured into ice-water (700 ml). The separated organic layer was washed with 1N hydrochloric acid and water, and dried over magnesium sulfate. The solvent was evaporated to give 1-(2-methylsulfonyloxyethyl)-4-ethoxycarbonyl-5-aminopyrazole (270.8 g) as crystals.

후처리

  1. temperaturecooling
  2. washThe separated organic layer was washed with 1N hydrochloric acid and water
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-abde1cb5470a442698c41ac1cbb3cfa2
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05366970

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