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Triethylamine → 2-(4-Ethoxycarbonylpiperidino)-4-(3,4-methylenedioxy-benzyl)amino-6-chloroquinazoline

HRID 1384910
ノート
印刷プレビュー

反応式

HRID 1384910 の反応式
[NH:1]1[CH2:10][CH2:9][CH:4]([C:5]([O:7][CH3:8])=[O:6])[CH2:3][CH2:2]1.[CH2:11](N(CC)CC)C.Cl[C:19]1[N:28]=[C:27]([NH:29][CH2:30][C:31]2[CH:36]=[CH:35][C:34]3[O:37][CH2:38][O:39][C:33]=3[CH:32]=2)[C:26]2[C:21](=[CH:22][CH:23]=[C:24]([Cl:40])[CH:25]=2)[N:20]=1>CC(O)C>[CH2:8]([O:7][C:5]([CH:4]1[CH2:9][CH2:10][N:1]([C:19]2[N:28]=[C:27]([NH:29][CH2:30][C:31]3[CH:36]=[CH:35][C:34]4[O:37][CH2:38][O:39][C:33]=4[CH:32]=3)[C:26]3[C:21](=[CH:22][CH:23]=[C:24]([Cl:40])[CH:25]=3)[N:20]=2)[CH2:2][CH2:3]1)=[O:6])[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

5

反応物 3

HCID 8471TriethylamineHCID 424914Methyl isonipecotateHCID 223398654-((1,3-Benzodioxol-5-ylmethyl)amino)-2,6-dichloro quinazoline

生成物 1

HCID 211838922-(4-Ethoxycarbonylpiperidino)-4-(3,4-methylenedioxy-benzyl)amino-6-chloroquinazoline収率 97.3%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

3.61 g of methyl isonipecotate, 2.32 g of triethylamine and 5 ml of 2-propanol were added to 1 g of 2,6-dichloro-4-(3,4-methylenedioxybenzyl)aminoquinazoline prepared in Example 92. The obtained mixture was refluxed for 100 minutes. The mixture thus obtained was extracted with chloroform twice. The organic layers were combined, washed with water, dried over magnesium sulfate and freed from the solvent by distillation. The residue was recrystallized (from ethanol/water) to give 1.31 g of the title compound.

後処理

  1. temperatureThe obtained mixture was refluxed for 100 minutes
  2. customThe mixture thus obtained
  3. extractionwas extracted with chloroform twice
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. distillationfreed from the solvent by distillation
  7. customThe residue was recrystallized (from ethanol/water)

出典と根拠

ORDレコード
ord-208732f781564035b2b3d5670c5e5ba5
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06262059B1

反応ノート

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