反応式
C(N(CC)CC)C.[CH:8]1([C:11](Cl)=[O:12])[CH2:10][CH2:9]1.[NH2:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]([N:24]2[CH2:33][C:32]3[CH:31]=[N:30][N:29]([CH3:34])[C:28]=3[NH:27][C:26]3[CH:35]=[C:36]([CH3:39])[CH:37]=[CH:38][C:25]2=3)=[O:23])=[CH:18][C:17]=1[CH3:40].CC1C=C2N=C3C(=NC(NC3=O)=O)N(C[C@H](O)[C@H](O)[C@H](O)CO)C2=CC=1C>ClCCl>[CH3:34][N:29]1[C:28]2[NH:27][C:26]3[CH:35]=[C:36]([CH3:39])[CH:37]=[CH:38][C:25]=3[N:24]([C:22]([C:19]3[CH:20]=[CH:21][C:16]([CH2:15][NH:14][C:11]([CH:8]4[CH2:10][CH2:9]4)=[O:12])=[C:17]([CH3:40])[CH:18]=3)=[O:23])[CH2:33][C:32]=2[CH:31]=[N:30]1参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
Triethylamine (0.145 ml, 1.04 mmol) and cyclopropanecarbonyl chloride (0.041 ml, 0.45 mmol) were added to a solution of (4-aminomethyl-3-methyl-phenyl)-(3,6-dimethyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulen-9-yl)-methanone from Example E101.2 (150 mg, 0.41 mmol) in dichloromethane (10 ml) at room temperature. The mixture was stirred for 20 h then concentrated in vacuo. The residue was purified by preparative HPLC (eluant; 0.5% 35% ammonia:9.5% methanol:90% dichloromethane) to give an off-white solid identified as the title compound (91 mg, 51%).
後処理
- customat room temperature
- concentrationthen concentrated in vacuo
- customThe residue was purified by preparative HPLC (eluant; 0.5% 35% ammonia:9.5% methanol:90% dichloromethane)
- customto give an off-white solid
出典と根拠
- ORDレコード
- ord-59d695f6394449a0a66d327c81572566
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08202858B2
関連ノート
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