Water → 4-(6,7-Dimethoxy-4-quinazolinyl)-N-[4-(piperidinomethyl)phenyl]-1-piperazinecarboxamide

HRID 993156노트

반응식

HRID 993156 반응식
Cl[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([N:12]2[CH2:17][CH2:16][N:15]([C:18]3[C:27]4[C:22](=[CH:23][C:24]([O:30][CH3:31])=[C:25]([O:28][CH3:29])[CH:26]=4)[N:21]=[CH:20][N:19]=3)[CH2:14][CH2:13]2)=[O:11])=[CH:5][CH:4]=1.[NH:32]1[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]1.O>CN(C)C=O>[CH3:29][O:28][C:25]1[CH:26]=[C:27]2[C:22](=[CH:23][C:24]=1[O:30][CH3:31])[N:21]=[CH:20][N:19]=[C:18]2[N:15]1[CH2:14][CH2:13][N:12]([C:10]([NH:9][C:6]2[CH:7]=[CH:8][C:3]([CH2:2][N:32]3[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]3)=[CH:4][CH:5]=2)=[O:11])[CH2:17][CH2:16]1

참가 물질

5

반응물 3

HCID 962WaterHCID 8082PiperidineHCID 22707657N-[4-(chloromethyl)phenyl]-4-(6,7-dimethoxy-4-quinazolinyl)-1-piperazinecarboxamide

생성물 1

HCID 227075284-(6,7-Dimethoxy-4-quinazolinyl)-N-[4-(piperidinomethyl)phenyl]-1-piperazinecarboxamide수율 92%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In 10 ml of toluene was suspended 593.5 mg (2.16 mmol) of 6,7-dimethoxy-4-piperazinylquinazoline obtained by the method described in South African Patent No. 67 06512 (1968), and 362.6 ml (2.16 mmol) of 4-(chloromethyl)phenyl isocyanate was added thereto, followed by stirring at room temperature for 3 hours. After the reaction mixture was filtered, the obtained crystals were washed with diisopropyl ether and dried under reduced pressure to give 916.8 mg (2.08 mmol, 96%) of N-[4-(chloromethyl)phenyl]-4-(6,7-dimethoxy-4-quinazolinyl)-1-piperazinecarboxamide. In 10 ml of dimethylformamide was dissolved 422.9 mg (0.96 mmol) of the obtained N-[4-(chloromethyl)phenyl]-4-(6,7-dimethoxy-4-quinazolinyl)-1-piperazinecarboxamide, and 0.28 ml (2.83 mmol) of piperidine was added thereto, followed by stirring at room temperature for 7 hours. Then, the reaction mixture was poured into water and the precipitated crystals were collected by filtration, followed by purification by silica gel column chromatography to give 430.9 mg (0.88 mmol) of the desired compound as colorless crystals.

후처리

  1. additionwas added
  2. filtrationthe precipitated crystals were collected by filtration
  3. customfollowed by purification by silica gel column chromatography

출처 및 근거

ORD 기록
ord-ed34b174bb3c4b6f9b7f7c311df8f15d
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06472391B2

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