Sec-Butylamine → HCID 19881217, 화합물

HRID 745308노트

반응식

HRID 745308 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16]([Cl:20])=[N:17][C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2.[CH:21]([NH2:25])([CH2:23][CH3:24])[CH3:22]>CN(C)C=O>[ClH:20].[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16]([NH:25][CH:21]([CH2:23][CH3:24])[CH3:22])=[N:17][C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2

참가 물질

4

반응물 2

HCID 24874Sec-ButylamineHCID 46787202-Chloro-6,7-dihydro-9,10-dimethoxy-4H-pyrimido[6,1-a]isoquinolin-4-one

생성물 1

HCID 19881217HCID 19881217, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 9,10-dimethoxy-6,7-dihydro-2-chloro-4H-pyrimido(6,1-a)isoquinolin-4-one (2.5 g), sec-butylamine (10 ml) and dimethylformamide (2 ml) is heated under reflux for 5 hours. The solvent and excess amine are distilled under reduced pressure. The residue is treated with water. A white solid precipitates and is collected by filtration. The precipitate is crystallized from methylene chloride-ether mixture, yield 2.10 g. The crystals are dissolved in dichloromethane and treated with a solution of etheral hydrochloric acid. The hydrochloride is crystallized from ethanol-ether mixture, m.p. 218°-225° C.

후처리

  1. temperatureunder reflux for 5 hours
  2. distillationThe solvent and excess amine are distilled under reduced pressure
  3. additionThe residue is treated with water
  4. customA white solid precipitates
  5. filtrationis collected by filtration
  6. customThe precipitate is crystallized from methylene chloride-ether mixture, yield 2.10 g
  7. dissolutionThe crystals are dissolved in dichloromethane
  8. additiontreated with a solution of etheral hydrochloric acid
  9. customThe hydrochloride is crystallized from ethanol-ether mixture, m.p. 218°-225° C.

출처 및 근거

ORD 기록
ord-e7d5709a5ff440d987630d6c477c43da
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04598148

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