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

HRID 2263164ノート

反応式

HRID 2263164 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-dccbff1734a342499fc3f758ec525e42
出典データセット
uspto-grants-2010_12
特許番号
US07851473B2

反応ノート

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