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Methanesulfonyl chloride → HCID 15077739, 화합물

HRID 1681650
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HRID 1681650 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-c60e1c548bb94208aee5401f59d90dc6
출처 데이터셋
uspto-grants-1992_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05173485

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