1-Fluoro-4-(1-isothiocyanatoethyl)benzene → HCID 10094291, 화합물

HRID 1352515노트

반응식

HRID 1352515 반응식
[CH2:1]([C:8]1[C:9]([C:13]2[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][CH:14]=2)=[N:10][O:11][CH:12]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F:20][C:21]1[CH:31]=[CH:30][C:24]([CH:25]([N:27]=[C:28]=[S:29])[CH3:26])=[CH:23][CH:22]=1>CN(C)C=O>[CH2:1]([C:8]1[C:9]([C:13]2[CH:14]=[CH:15][C:16]([NH:19][C:28]([NH:27][CH:25]([C:24]3[CH:23]=[CH:22][C:21]([F:20])=[CH:31][CH:30]=3)[CH3:26])=[S:29])=[CH:17][CH:18]=2)=[N:10][O:11][CH:12]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 5195361-Fluoro-4-(1-isothiocyanatoethyl)benzeneHCID 21100737HCID 21100737, 화합물

생성물 1

HCID 10094291HCID 10094291, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 4-(4-benzyl-isoxazol-3-yl)-phenylamine and 4-fluoro-α-methyl-benzyl isothiocyanate in dimethylformamide (5 mL) is stirred for 12 hours at room temperature. The reaction mixture is then partitioned between ethyl acetate and water. The organic layer is washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 1.4 g crude product as a yellow solid. The latter is recrystallized from ethyl acetate/hexane to give 0.9 g product as a yellow solid. MS: m/z 433 (M+H)+.

후처리

  1. customThe reaction mixture is then partitioned between ethyl acetate and water
  2. washThe organic layer is washed with saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give 1.4 g crude product as a yellow solid
  6. customThe latter is recrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-1776ada67fe54e45ae9af346f1806bc4
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07220768B2

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