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

HRID 992251

反応式

HRID 992251 の反応式
[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

参加物

6

反応物 2

HCID 6621SulphenoneHCID 24654Hydrazine hydrate (1:1)

生成物 1

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

試薬・触媒・溶媒 3

HCID 8471Triethylamine触媒HCID 174Ethylene Glycol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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°

出典と根拠

ORDレコード
ord-9f7b3e5a9568410fb0b08494e650a7a6
出典データセット
uspto-grants-2002_10
特許番号
US06468999B1

関連ノート

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