Hydrazine → p-Hydrazinobenzenesulphonamide

HRID 8081

反応式

HRID 8081 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[NH2:12][NH2:13]>O>[NH:12]([C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1)[NH2:13]

参加物

4

反応物 2

HCID 9321HydrazineHCID 668244-Chlorobenzenesulfonamide

生成物 1

HCID 78105p-Hydrazinobenzenesulphonamide収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A stirred solution of 4-chlorobenzenesulfonamide (38.33 g, 200 mmol) and anhydrous hydrazine (31.4 mL, 1.0 mol) was heated at reflux for 30 hours. After cooling to room temperature, the mixture was poured into water (500 mL) with swirling. The resulting precipitate was collected by filtration, washed thoroughly with water several times, air-dried, and dried under vacuum to give the title compound (35.5 g, 95% yield) as a white solid. Mp 169–171° C. 1H NMR (300 MHz, THF-d8) δ 7.59 (d, J=8.8 Hz, 2H), 6.77 (d, J=8.8 Hz, 2H), 6.62 (br, 1H), 5.99 (br, 2H), 3.87 (br, 2H). Mass spectrum (API-TIS) m/z 188 (MH+).

後処理

  1. temperatureat reflux for 30 hours
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed thoroughly with water several times
  4. customair-dried
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-4f84ead693da4f968cd28a52005d8455
出典データセット
uspto-grants-2006_08
特許番号
US07087630B2

関連ノート

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