Hydrochloric Acid → HCID 20506459, 화합물

HRID 1577327노트

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HRID 1577327 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[C:7]([O:15][CH3:16])[C:8]([O:13][CH3:14])=[C:9]([Cl:12])[CH:10]=2)[N:5]=[C:4](Cl)[N:3]=1.[CH2:18]([O:20][CH2:21][CH2:22][O:23][CH:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1)[CH3:19].C(N(CC)CC)C.Cl>C(O)CCC.C(O)C>[ClH:12].[CH2:18]([O:20][CH2:21][CH2:22][O:23][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:15][CH3:16])[C:8]([O:13][CH3:14])=[C:9]([Cl:12])[CH:10]=3)[N:5]=2)[CH2:26][CH2:25]1)[CH3:19]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 12920006HCID 12920006, 화합물HCID 140223854-(2-Ethoxyethoxy)piperidine

생성물 1

HCID 20506459HCID 20506459, 화합물

시약·촉매·용매 2

HCID 2631-Butanol용매HCID 702Ethanol용매

실험 절차

4-Amino-2,6-dichloro-7,8-dimethoxyquinazoline (4.9 g.), 4-(2-ethoxyethoxy)piperidine (3.2 g.) and triethylamine (10 ml.) in n-butanol (400 ml.) are heated at reflux overnight under an atmosphere of nitrogen. The mixture is then cooled, evaporated in vacuo, and the residue basified (aqueous Na2CO3) and extracted 3 times with chloroform. The combined chloroform extracts are evaporated and the residue chromatographed on neutral alumina to give the crude product which is converted to the hydrochloride salt by treatment with hydrogen chloride in ethanol to afford the title compound.

후처리

  1. temperatureat reflux overnight under an atmosphere of nitrogen
  2. temperatureThe mixture is then cooled
  3. customevaporated in vacuo
  4. extractionextracted 3 times with chloroform
  5. customThe combined chloroform extracts are evaporated
  6. customthe residue chromatographed on neutral alumina
  7. customto give the crude product which

출처 및 근거

ORD 기록
ord-11f1daed6e734ba9b1de2411bd6c8b37
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04287341

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