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Water → HCID 22316751, 화합물

HRID 396769
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HRID 396769 반응식
[F:1][CH2:2][S:3]([C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][CH:7]=1)(=[O:5])=[O:4].[NH2:13][NH2:14].O.Cl.CO>CN(C=O)C>[ClH:12].[F:1][CH2:2][S:3]([C:6]1[CH:11]=[CH:10][C:9]([NH:13][NH2:14])=[CH:8][CH:7]=1)(=[O:5])=[O:4]
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참가 물질

6

반응물 4

HCID 962WaterHCID 9321HydrazineHCID 21893726Hydrochloride methanolHCID 22316655HCID 22316655, 화합물

생성물 1

HCID 22316751HCID 22316751, 화합물수율 49.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 4-chlorophenyl fluoromethyl sulfone (1.97 g, 9.44 mmol. prepared according to the method of Ukrainskill Khimicheskill Zhurnal, 1972, 38. 1034) and hydrazine anhydrous (1.84 g, 57.5 mmol) in DMF (30 mL) was heated to 120° C. for 16 hours, and cooled down to room temperature. The reaction mixture was poured into water (150 mL) and the whole was extracted with ethyl acetate/hexane/ether (2/1/1, 60 mL×3). The organic layer was washed with brine, dried over sodium sulfate, and concentrated in vacuo. The resulting solid (1.56 g, 7.64 mmol) was added HCl-MeOH reagent 10 (10 mL) at room temperature and stirred for 10 minutes. The mixture was concentrated in vacuo to give the subtitle compound (0.91 g, 49.4% yield).

후처리

  1. customprepared
  2. extractionthe whole was extracted with ethyl acetate/hexane/ether (2/1/1, 60 mL×3)
  3. washThe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. concentrationThe mixture was concentrated in vacuo

출처 및 근거

ORD 기록
ord-f9c2e37fb5d24c36a23ff17e75857d14
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06608095B2

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