Triethylamine → HCID 20351360、化合物

HRID 1448952ノート

反応式

HRID 1448952 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.[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

参加物

5

反応物 3

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

生成物 1

HCID 20351360HCID 20351360、化合物収率 88%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2e8b6097bbd24989b8de0ccb073d3844
出典データセット
uspto-grants-1980_02
特許番号
US04188391

反応ノート

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