Water → 2,2,2-Trichloroethyl (1,3-dimethyl-1H-pyrazol-5-yl)carbamate

HRID 2263164노트

반응식

HRID 2263164 반응식
[CH3:1][N:2]1[C:6]([NH2:7])=[CH:5][C:4]([CH3:8])=[N:3]1.Cl[C:10]([O:12][CH2:13][C:14]([Cl:17])([Cl:16])[Cl:15])=[O:11].O>CC(N(C)C)=O>[CH3:1][N:2]1[C:6]([NH:7][C:10](=[O:11])[O:12][CH2:13][C:14]([Cl:17])([Cl:16])[Cl:15])=[CH:5][C:4]([CH3:8])=[N:3]1

참가 물질

5

반응물 3

HCID 962WaterHCID 870632,2,2-Trichloroethyl chloroformateHCID 5207211,3-Dimethyl-1H-pyrazol-5-amine

생성물 1

HCID 866255062,2,2-Trichloroethyl (1,3-dimethyl-1H-pyrazol-5-yl)carbamate수율 40.8%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

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온도
0 °C

실험 절차

To a solution of 1,3-dimethyl-1H-pyrazol-5-amine (500 mg, 4.50 mmol) in dimethylacetamide (15 ml) was added 2,2,2-trichloroethyl chloroformate (0.747 ml, 5.40 mmol) with ice-cooling, and the mixture was stirred at 0° C. for 1 hour. Water was poured into the reaction solution, and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) to give 526 mg (40.8%) of the desired product as an oil.

후처리

  1. temperaturecooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-dccbff1734a342499fc3f758ec525e42
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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