Thionyl Chloride → HCID 178514949, 화합물

HRID 1076713노트

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HRID 1076713 반응식
S(Cl)([Cl:3])=O.O[CH2:6][CH2:7][CH2:8][NH:9][C:10]1[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)([OH:19])[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]=1>C(Cl)(Cl)Cl>[Cl:3][CH2:6][CH2:7][CH2:8][NH:9][C:10]1[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)([OH:19])[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]=1

참가 물질

4

실험 절차

Thionylchloride (1.53 ml.) was added dropwise to a stirred cooled suspension of 2-(3-hydroxypropylamino)-3-phenyl-3H-indol-3-ol (3 g.) in chloroform (25 ml.). On completion of the addition the reaction was allowed to warm to room temperature and then heated under reflux for 45 minutes. The solvent and excess thionyl chloride were removed under reduced pressure and the resulting product crystallised from isopropanol-ether to give the title compound as its hydrochloride salt (2.72 g.). After two recrystallisations from isopropanol-ether the hydrochloride had a m.p. 210°-212°C. (Found C, 60.8; H. 5.6; N, 8.3. C17H17ClN20HCl requires C, 60.5; H, 5.4; N 8.3%).

후처리

  1. temperaturecooled
  2. additionOn completion of the addition the reaction
  3. temperatureheated
  4. temperatureunder reflux for 45 minutes
  5. customThe solvent and excess thionyl chloride were removed under reduced pressure
  6. customthe resulting product crystallised from isopropanol-ether

출처 및 근거

ORD 기록
ord-8f6710b7b2e74269af44a2a8ee29aebb
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03957819

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