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Hydrazine → HCID 178514377, 화합물

HRID 897882
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HRID 897882 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[F:17])=S)=[CH:4][CH:3]=1.[NH2:18][NH2:19]>C(O)C.O1CCCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[F:17])=[N:18][NH2:19])=[CH:4][CH:3]=1
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참가 물질

5

반응물 2

HCID 9321Hydrazine2회HCID 22346994HCID 22346994, 화합물

생성물 1

HCID 178514377HCID 178514377, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매2회

실험 절차

N1-(4-bromophenyl)-2-fluoro-1-benzenecarbothioamide (1.50 g, 0.00485 mol) and a 1M solution of hydrazine in tetrahydrofuran (6.3 mL, 0.0063 mol) were heated in absolute ethanol (25 mL) at reflux under nitrogen atmosphere for 14 hours. Additional 3 mL of a 1M solution of hydrazine in tetrahydrofuran was added and the stirring at reflux was continued for another 6 hours. The reaction mixture was cooled to ambient temperature, the solvent was removed under reduced pressure and the residue partitioned between saturated solution of sodium bicarbonate in water (50 mL) and ethyl acetate (50 mL). The organic phase was washed with brine, dried with magnesium sulfate and concentrated to yield N1-(4-bromophenyl)-2-fluoro-1-benzenecarbohydrazonamide (1.54 g, 0.0050 mol) as a tan solid. TLC (ethyl acetate/heptane 1:3) Rf 0.10.

후처리

  1. temperatureat reflux under nitrogen atmosphere for 14 hours
  2. temperaturethe stirring at reflux
  3. customthe solvent was removed under reduced pressure
  4. customthe residue partitioned between saturated solution of sodium bicarbonate in water (50 mL) and ethyl acetate (50 mL)
  5. washThe organic phase was washed with brine
  6. dry with materialdried with magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-cbd6a40a301c4f92908b9733dcf0ba7c
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06921763B2

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