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

HRID 353133

반응식

HRID 353133 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bb64dae8372d4097a20658a543248991
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06750218B2

연결된 노트

불러오는 중…