Water → 1-[4-Phenyl-5-(phenylthio)-1,3-thiazol-2-yl]methanamine

HRID 2359956노트

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HRID 2359956 반응식
[C:1]1([C:7]2[N:8]=[C:9]([CH2:19][N:20]3C(=O)C4C(=CC=CC=4)C3=O)[S:10][C:11]=2[S:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.NN.O>C(O)C>[C:1]1([C:7]2[N:8]=[C:9]([CH2:19][NH2:20])[S:10][C:11]=2[S:12][C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 576877262-{[4-phenyl-5-(phenylthio)-1,3-thiazol-2-yl]methyl}-1H-isoindole-1,3(2H)-dione

생성물 1

HCID 576877291-[4-Phenyl-5-(phenylthio)-1,3-thiazol-2-yl]methanamine수율 97.5%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
70 °C

실험 절차

To a suspension of 2-{[4-phenyl-5-(phenylthio)-1,3-thiazol-2-yl]methyl}-1H-isoindole-1,3(2H)-dione (0.53 g) in ethanol (5 mL) was added hydrazine monohydrate (0.1 mL), and the mixture was stirred at 70° C. for 1 hr. The reaction mixture was cooled to room temperature, water was added, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution, water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give the title compound as a yellow oil (yield 0.36 g, 97%).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with saturated aqueous sodium hydrogen carbonate solution, water and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-4bacd34aeb74474cb18ee56e4fb4e81f
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08686010B2

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