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

HRID 1533126ノート

反応式

HRID 1533126 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][N:7]=[C:6]2[N:15]1[CH2:20][CH2:19][N:18]([C:21]([NH2:23])=[O:22])[CH2:17][CH2:16]1.[NH:24]1[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1.O>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][N:7]=[C:6]2[N:15]1[CH2:20][CH2:19][N:18]([C:21]([NH:23][C:12]2[CH:11]=[CH:10][C:5]([CH2:6][N:24]3[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]3)=[CH:4][CH:3]=2)=[O:22])[CH2:17][CH2:16]1

参加物

5

反応物 3

HCID 962WaterHCID 8082PiperidineHCID 86756553HCID 86756553、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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-l4-(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.

後処理

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

出典と根拠

ORDレコード
ord-6f9a2203487b476b98556d1be7f0a77f
出典データセット
uspto-grants-2001_03
特許番号
US06207667B1

反応ノート

読み込み中…