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

HRID 2263066

반응식

HRID 2263066 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-380a2c4ef7df493c814a5bcd7cecbb02
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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