Di-tert-butyl dicarbonate → 4-(6,7-Dimethoxy-4-quinazolinyl)-N-(3-isopropylphenyl)-1-piperazinecarboxamide

HRID 353133

反応式

HRID 353133 の反応式
[C:1](OC(OC(C)(C)C)=O)(OC(C)(C)C)=[O:2].[CH:16]([C:19]1[CH:20]=[C:21]([CH:23]=[CH:24][CH:25]=1)[NH2:22])([CH3:18])[CH3:17].[CH3:26][O:27][C:28]1[CH:29]=[C:30]2[C:35](=[CH:36][C:37]=1[O:38][CH3:39])[N:34]=[CH:33][N:32]=[C:31]2[N:40]1[CH2:45][CH2:44][NH:43][CH2:42][CH2:41]1>ClCCl.CN(C1C=CN=CC=1)C>[CH3:26][O:27][C:28]1[CH:29]=[C:30]2[C:35](=[CH:36][C:37]=1[O:38][CH3:39])[N:34]=[CH:33][N:32]=[C:31]2[N:40]1[CH2:41][CH2:42][N:43]([C:1]([NH:22][C:21]2[CH:23]=[CH:24][CH:25]=[C:19]([CH:16]([CH3:18])[CH3:17])[CH:20]=2)=[O:2])[CH2:44][CH2:45]1

参加物

6

反応物 3

HCID 90495Di-tert-butyl dicarbonateHCID 4586793-IsopropylanilineHCID 27584846,7-Dimethoxy-4-piperazin-1-yl-quinazoline

生成物 1

HCID 227074514-(6,7-Dimethoxy-4-quinazolinyl)-N-(3-isopropylphenyl)-1-piperazinecarboxamide収率 63%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2.05 g (9.39 mmol) of di-tert-butyl dicarbonate in 30 ml of dichloromethane was added 108 mg (0.88 mmol) of 4-(N,N-dimethylamino)pyridine. After the mixture was stirred at room temperature for 5 minutes, 1.26 ml (8.95 mmol) of 3-isopropylaniline was added thereto, followed by further stirring at room temperature for 30 minutes. To the reaction mixture was added 548 mg (2.00 mmol) of 6,7-dimethoxy-4-piperazinylquinazoline obtained by the method described in South African Patent No. 67 06512 (1968), followed by stirring at room temperature for 30 minutes. After the solvent was evaporated, the residue was purified by silica gel chromatography and recrystallized from ethyl acetate to give the desired compound as colorless crystals.

後処理

  1. stirringby further stirring at room temperature for 30 minutes
  2. customobtained by the method
  3. stirringby stirring at room temperature for 30 minutes
  4. customAfter the solvent was evaporated
  5. customthe residue was purified by silica gel chromatography
  6. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-bb64dae8372d4097a20658a543248991
出典データセット
uspto-grants-2004_06
特許番号
US06750218B2

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