Triethylamine → 6,7-dimethoxy-2-[5-(4-methyl-piperazine-1-sulfonyl)-3,4-dihydro-1H-isoquinolin-2-yl]-3H-quinazolin-4-one

HRID 2183704

反応式

HRID 2183704 の反応式
Cl[C:2]1[NH:11][C:10](=[O:12])[C:9]2[C:4](=[CH:5][C:6]([O:15][CH3:16])=[C:7]([O:13][CH3:14])[CH:8]=2)[N:3]=1.[CH3:17][N:18]1[CH2:23][CH2:22][N:21]([S:24]([C:27]2[CH:36]=[CH:35][CH:34]=[C:33]3[C:28]=2[CH2:29][CH2:30][NH:31][CH2:32]3)(=[O:26])=[O:25])[CH2:20][CH2:19]1.C(N(CC)CC)C>CS(C)=O.O>[CH3:14][O:13][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][C:6]=1[O:15][CH3:16])[N:3]=[C:2]([N:31]1[CH2:30][CH2:29][C:28]3[C:33](=[CH:34][CH:35]=[CH:36][C:27]=3[S:24]([N:21]3[CH2:20][CH2:19][N:18]([CH3:17])[CH2:23][CH2:22]3)(=[O:26])=[O:25])[CH2:32]1)[NH:11][C:10]2=[O:12]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 219836535-(4-Methyl-piperazine-1-sulfonyl)-1,2,3,4-tetrahydro-isoquinolineHCID 1354566642-Chloro-6,7-dimethoxy-3H-quinazolin-4-one

生成物 1

HCID 1360113286,7-dimethoxy-2-[5-(4-methyl-piperazine-1-sulfonyl)-3,4-dihydro-1H-isoquinolin-2-yl]-3H-quinazolin-4-one収率 37.2%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

A mixture of 2-chloro-6,7-dimethoxy-3H-quinazolin-4-one 1b, (0.77 g, 3.23 mmol), 5-(4-methyl-piperazine-1-sulfonyl)-1,2,3,4-tetrahydro-isoquinoline 11a (1.25 g, 3.41 mmol) and triethylamine (0.75 g, 1.04 mL, 7.46 mmol) in DMSO (15 mL) was heated at 80° C. with stirring for 18 h. After cooling to room temperature the reaction was diluted with water. The precipitated white product was collected by filtration, washed with water, and dried to give 0.6 g of 6,7-dimethoxy-2-[5-(4-methyl-piperazine-1-sulfonyl)-3,4-dihydro-1H-isoquinolin-2-yl]-3H-quinazolin-4-one 401, mp. 230-237° C.

後処理

  1. temperatureAfter cooling to room temperature the reaction
  2. filtrationThe precipitated white product was collected by filtration
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-1a02fd9b6cfd4f12bf4e4557b49327e7
出典データセット
uspto-grants-2005_05
特許番号
US06900220B2

関連ノート

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