Pyridine → 2,2,2-Trichloroethyl (3-phenylisoxazol-5-yl)carbamate

HRID 2263066

反応式

HRID 2263066 の反応式
[C:1]1([C:7]2[CH:11]=[C:10]([NH2:12])[O:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.N1C=CC=CC=1.Cl[C:20]([O:22][CH2:23][C:24]([Cl:27])([Cl:26])[Cl:25])=[O:21]>O1CCCC1>[C:1]1([C:7]2[CH:11]=[C:10]([NH:12][C:20](=[O:21])[O:22][CH2:23][C:24]([Cl:27])([Cl:26])[Cl:25])[O:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 870632,2,2-Trichloroethyl chloroformateHCID 2612015-Amino-3-phenylisoxazole

生成物 1

HCID 862452722,2,2-Trichloroethyl (3-phenylisoxazol-5-yl)carbamate収率 85.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 3-phenylisoxazole-5-amine (420 mg, 2.62 mmol) and pyridine (0.636 ml, 7.87 mmol) in tetrahydrofuran (5 ml) was added 2,2,2-trichloroethyl chloroformate (0.542 ml, 3.93 mmol) with ice-cooling, the mixture was stirred for 30 minutes with ice-cooling, the reaction mixture was poured into ice-water 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 to obtain the desired product (750 mg, 85.3%) as a solid.

後処理

  1. temperaturecooling
  2. temperaturecooling
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-380a2c4ef7df493c814a5bcd7cecbb02
出典データセット
uspto-grants-2010_12
特許番号
US07851473B2

関連ノート

読み込み中…