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

HRID 1414576노트

반응식

HRID 1414576 반응식
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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-074f683bb77c4dde8950488fef0c78a2
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04001422

반응 노트

불러오는 중…