Hydrazine → p-Hydrazinobenzenesulphonamide

HRID 8081

반응식

HRID 8081 반응식
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]

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 668244-Chlorobenzenesulfonamide

생성물 1

HCID 78105p-Hydrazinobenzenesulphonamide수율 95%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-4f84ead693da4f968cd28a52005d8455
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07087630B2

연결된 노트

불러오는 중…