Triethylamine → HCID 20351360, 화합물

HRID 1448952노트

반응식

HRID 1448952 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.[CH3:17][S:18]([NH:21][CH2:22][CH2:23][CH:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1)(=[O:20])=[O:19].C(N(CC)CC)C>C(O)C>[CH3:13][O:12][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][C:8]=1[O:14][CH3:15])[N:5]=[CH:4][N:3]=[C:2]2[N:27]1[CH2:26][CH2:25][CH:24]([CH2:23][CH2:22][NH:21][S:18]([CH3:17])(=[O:20])=[O:19])[CH2:29][CH2:28]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27693644-Chloro-6,7-dimethoxyquinazolineHCID 20511180N-[2-(Piperidin-4-yl)ethyl]methanesulfonamide--hydrogen chloride (1/1)

생성물 1

HCID 20351360HCID 20351360, 화합물수율 88%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4-Chloro-6,7-dimethoxy quinazoline (1.1 g.), 4- (2-methanesulphonamidoethyl)piperidine hydrochloride (1.5 g.) and triethylamine (1.5 ml.) in ethanol (30 ml.) were heated together under reflux for 1.5 hours. The solution was then cooled to room temperature, concentrated in vacuo, suspended in water (70 ml.) and basified to pH 10 with 10% aqueous sodium carbonate solution. The mixture was extracted with chloroform (2×70 ml.), the extracts combined, dried (MgSO4), and taken to dryness in vacuo. The resultant pale yellow oil was triturated with ether (70 ml.) to give a white solid which was collected by filtration. Crystallization of this solid from ethanol yielded 6,7-dimethoxy-4-[4-(2-methanesulphonamidoethyl)-piperidino]quinazoline (1.7 g.), m.p. 162°-164° C.

후처리

  1. temperatureunder reflux for 1.5 hours
  2. concentrationconcentrated in vacuo
  3. extractionThe mixture was extracted with chloroform (2×70 ml.)
  4. dry with materialdried (MgSO4)
  5. customThe resultant pale yellow oil was triturated with ether (70 ml.)
  6. customto give a white solid which
  7. filtrationwas collected by filtration
  8. customCrystallization of this solid from ethanol

출처 및 근거

ORD 기록
ord-2e8b6097bbd24989b8de0ccb073d3844
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04188391

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