Isoamyl Alcohol → 2-(4-Benzylpiperidin-1-yl)-4-amino-7,8-dimethoxyquinazoline hydrochloride

HRID 1577322노트

반응식

HRID 1577322 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[CH:9][CH:10]=2)[N:5]=[C:4]([Cl:16])[N:3]=1.[CH2:17]([CH:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(O)CC(C)C>C(OCC)C>[ClH:16].[CH2:17]([CH:24]1[CH2:29][CH2:28][N:27]([C:4]2[N:3]=[C:2]([NH2:1])[C:11]3[C:6](=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[CH:9][CH:10]=3)[N:5]=2)[CH2:26][CH2:25]1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 31260Isoamyl AlcoholHCID 317384-BenzylpiperidineHCID 129200082-Chloro-4-amino-7,8-dimethoxyquinazoline

생성물 1

HCID 205064012-(4-Benzylpiperidin-1-yl)-4-amino-7,8-dimethoxyquinazoline hydrochloride수율 60%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

4-Amino-2-chloro-7,8-dimethoxyquinazoline (2.40 g., 10 mmole), 4-benzylpiperidine (1.93 g., 11 mmole) and 50 ml. of isoamyl alcohol were heated at reflux under a nitrogen atmosphere for two hours and cooled to room temperature. Diethyl ether (50 ml.) was added and the mixture allowed to stand in the refrigerator for two days. The precipitated solid was collected by filtration and recrystallized from ethanol/diethyl ether to afford 2.50 g. (60%) of the title compound, M.P. 216°-217° C.

후처리

  1. temperatureat reflux under a nitrogen atmosphere for two hours
  2. filtrationThe precipitated solid was collected by filtration
  3. customrecrystallized from ethanol/diethyl ether
  4. customto afford 2.50 g

출처 및 근거

ORD 기록
ord-b9df01931ff640748e40147d4a8585be
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04287341

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