Sec-Butylamine → HCID 19881217、化合物

HRID 745308ノート

反応式

HRID 745308 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 19881217HCID 19881217、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-e7d5709a5ff440d987630d6c477c43da
出典データセット
uspto-grants-1986_07
特許番号
US04598148

反応ノート

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