Sulphenone → Hydrazine, (4-(phenylsulfonyl)phenyl)-

HRID 992251

반응식

HRID 992251 반응식
[C:1]1([S:7]([C:10]2[CH:15]=[CH:14][C:13](Cl)=[CH:12][CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.[NH2:18][NH2:19]>C(N(CC)CC)C.C(O)CO.O>[C:1]1([S:7]([C:10]2[CH:15]=[CH:14][C:13]([NH:18][NH2:19])=[CH:12][CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 2

HCID 6621SulphenoneHCID 24654Hydrazine hydrate (1:1)

생성물 1

HCID 116834Hydrazine, (4-(phenylsulfonyl)phenyl)-

시약·촉매·용매 3

HCID 8471Triethylamine촉매HCID 174Ethylene Glycol용매HCID 962Water용매

실험 절차

A mixture of 4-chlorophenyl phenyl sulfone (10.1 g, 40.0 mmol), hydrazine mono-hydrate (30 mL), and triethylamine (4 drops) in ethylene glycol (20 mL) is heated at 150° for 15 hr. Upon cooling, the mixture is diluted with H2O and filtered. The residual solid is washed with H2O until the washings are neural (pH=6). This material is then triturated with methylene chloride and dried under reduced pressure at 50° to give the title compound, IR (drift) 3282, 1586, 1514, 1306, 1291, 1158, 1145, 1104, 996, 813, 756, 730, 717, 688 and 678 cm−1; NMR (300 MHz, CDCl3) 7.70-7.85, 7.45-7.65, 6.79 and 4.22 δ; MS (EI) m/z 248 (M+), 125, 123, 108, 107, 90, 80, 77, 63 and 51.

후처리

  1. temperatureis heated at 150° for 15 hr
  2. temperatureUpon cooling
  3. filtrationfiltered
  4. washThe residual solid is washed with H2O until the washings
  5. customThis material is then triturated with methylene chloride
  6. customdried under reduced pressure at 50°

출처 및 근거

ORD 기록
ord-9f7b3e5a9568410fb0b08494e650a7a6
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06468999B1

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