Hydrochloric Acid → HCID 20506459、化合物

HRID 1577327ノート

反応式

HRID 1577327 の反応式
[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]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 12920006HCID 12920006、化合物HCID 140223854-(2-Ethoxyethoxy)piperidine

生成物 1

HCID 20506459HCID 20506459、化合物

試薬・触媒・溶媒 2

HCID 2631-Butanol溶媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-11f1daed6e734ba9b1de2411bd6c8b37
出典データセット
uspto-grants-1981_09
特許番号
US04287341

反応ノート

読み込み中…