Water → 4-(6,7-Dimethoxy-4-quinazolinyl)-N,N-diphenyl-1-piperazinecarboxamide

HRID 353129

反応式

HRID 353129 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][NH:18][CH2:17][CH2:16]1.C(N(CC)CC)C.[C:28]1([N:34]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[C:35](Cl)=[O:36])[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=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[CH2:16][CH2:17][N:18]([C:35]([N:34]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)=[O:36])[CH2:19][CH2:20]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 65741N,N-Diphenylcarbamic chlorideHCID 27584846,7-Dimethoxy-4-piperazin-1-yl-quinazoline

生成物 1

HCID 227076154-(6,7-Dimethoxy-4-quinazolinyl)-N,N-diphenyl-1-piperazinecarboxamide収率 99.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In 10 ml of dimethylformamide was dissolved 400 mg (1.46 mmol) of 6,7-dimethoxy-4-piperazinylquinazoline obtained according to the method described in South African Patent No. 67 06512 (1968), and 1.02 ml (7.32 mmol) of triethylamine was added thereto. To the resulting mixture was added 406 mg (1.75 mmol) of diphenylcarbamoyl chloride, followed by overnight stirring at room temperature. After the reaction mixture was poured into water, the precipitated crystals were collected by filtration, followed by purification by silica gel column chromatography to give 680 mg of the desired compound as colorless crystals.

後処理

  1. customobtained
  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-8ec0e79306154fc0b0eef1e7427fd64e
出典データセット
uspto-grants-2004_06
特許番号
US06750218B2

関連ノート

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