Hydrochloric Acid → HCID 20506459、化合物

HRID 354818ノート

反応式

HRID 354818 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. C. By the above procedures the following compounds are similarly provided from the appropriate starting materials in each case.

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-d6f6acc30cc44fcaa2478df6c63a6b86
出典データセット
uspto-grants-1983_03
特許番号
US04377581

反応ノート

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