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Isopropanol → 2-[N-(3-Ethoxycarbonylpropyl)-N-methylamino]-4-(3,4-methylenedioxybenzyl)amino-6-cyanoquinazoline

HRID 1938549
ノート
印刷プレビュー

反応式

HRID 1938549 の反応式
Cl.[CH3:2][NH:3][CH2:4][CH2:5][CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8].C(N(CC)CC)C.CC(O)C.Cl[C:24]1[N:33]=[C:32]([NH:34][CH2:35][C:36]2[CH:41]=[CH:40][C:39]3[O:42][CH2:43][O:44][C:38]=3[CH:37]=2)[C:31]2[C:26](=[CH:27][CH:28]=[C:29]([C:45]#[N:46])[CH:30]=2)[N:25]=1>CN(C)C=O>[CH2:10]([O:9][C:7]([CH2:6][CH2:5][CH2:4][N:3]([C:24]1[N:33]=[C:32]([NH:34][CH2:35][C:36]2[CH:41]=[CH:40][C:39]3[O:42][CH2:43][O:44][C:38]=3[CH:37]=2)[C:31]2[C:26](=[CH:27][CH:28]=[C:29]([C:45]#[N:46])[CH:30]=2)[N:25]=1)[CH3:2])=[O:8])[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3776IsopropanolHCID 8471TriethylamineHCID 14177893Ethyl 4-(methylamino)butanoate hydrochlorideHCID 211839842-Chloro-4-(3,4-methylenedioxybenzyl)amino-6-cyanoquinazoline

生成物 1

HCID 220693432-[N-(3-Ethoxycarbonylpropyl)-N-methylamino]-4-(3,4-methylenedioxybenzyl)amino-6-cyanoquinazoline収率 77.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

858 mg of ethyl N-methyl-4-aminobutyrate hydrochloride, 238 mg of triethylamine, 4 ml of 2-propanol and 2 ml of N,N-dimethylformamide were added to 400 mg of 2-chloro-4-(3,4-methylenedioxybenzyl)amino-6-cyanoquinazoline. The obtained mixture was refluxed for 1 hour, cooled to room temperature and filtered. The filtrate was distilled under a reduced pressure to remove the solvent and the residue was recrystallized (from ethanol/water) to give 410 mg of the title compound.

後処理

  1. temperatureThe obtained mixture was refluxed for 1 hour
  2. filtrationfiltered
  3. distillationThe filtrate was distilled under a reduced pressure
  4. customto remove the solvent
  5. customthe residue was recrystallized (from ethanol/water)

出典と根拠

ORDレコード
ord-79f23b7fb99d4a8eac82ab1834ba6f01
出典データセット
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05693652

反応ノート

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