Triethylamine → 1-(6,7-Dimethoxy-4-quinazolinyl)-4-piperidinone

HRID 1414576ノート

反応式

HRID 1414576 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[CH:4][N:3]=1.Cl.C1O[C:20]2([CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)[O:19]C1.C(N(CC)CC)C.C(=O)([O-])[O-].[Na+].[Na+]>Cl.C(O)C>[O:19]=[C:20]1[CH2:25][CH2:24][N:23]([C:2]2[C:11]3[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=3)[N:5]=[CH:4][N:3]=2)[CH2:22][CH2:21]1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 10340Sodium CarbonateHCID 27693644-Chloro-6,7-dimethoxyquinazolineHCID 162187951,4-Dioxa-8-azaspiro(4.5)decane hydrochloride

生成物 1

HCID 147388231-(6,7-Dimethoxy-4-quinazolinyl)-4-piperidinone収率 98%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

4-Chloro-6,7-dimethoxyquinazoline (30 g), 4-piperidone ethylene ketal hydrochloride (25 g), triethylamine (35 g) and ethanol (250 ml.) were refluxed together for 3 hours. Aqueous sodium carbonate was added followed by extraction with chloroform after which the chloroform extract was dried and evaporated in vacuo to give an oil. The oil was redissolved in aqueous hydrochloric acid (1.5N, 200 ml.) and refluxed for 2 hours followed by cooling, basification (Na2CO3 10% soln) and extraction into chlororform. Evaporation of the dried chloroform extract gave 4-(4-oxo-piperidino)-6,7-dimethoxyquinazoline (37.6 g) m.p. 176°-8° C.

後処理

  1. extractionfollowed by extraction with chloroform after which the chloroform
  2. extractionextract
  3. customwas dried
  4. customevaporated in vacuo
  5. customto give an oil
  6. temperaturerefluxed for 2 hours
  7. temperatureby cooling
  8. extractionbasification (Na2CO3 10% soln) and extraction into chlororform
  9. customEvaporation of the dried chloroform
  10. extractionextract

出典と根拠

ORDレコード
ord-074f683bb77c4dde8950488fef0c78a2
出典データセット
uspto-grants-1977_01
特許番号
US04001422

反応ノート

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