Isocyanate → HCID 10573917、化合物
反応式
[Br:1][C:2]1[CH:3]=[C:4](C(N=[N+]=[N-])=O)[CH:5]=[N:6][CH:7]=1.[N-:13]=[C:14]=[O:15].[CH3:16][O:17][C:18]1[CH:19]=[C:20]2[C:24](=[CH:25][C:26]=1[C:27]([F:30])([F:29])[F:28])[NH:23][CH2:22][CH2:21]2>C1(C)C=CC=CC=1.ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([NH:13][C:14]([N:23]2[C:24]3[C:20](=[CH:19][C:18]([O:17][CH3:16])=[C:26]([C:27]([F:29])([F:30])[F:28])[CH:25]=3)[CH2:21][CH2:22]2)=[O:15])[CH:5]=[N:6][CH:7]=1参加物
6
実験手順
5-Bromo-3-pyridylcarbonylazide (3.7 g, 16 mmoles) was heated under reflux in dry toluene (100 ml) for 1 hr. After cooling the resulting solution of isocyanate was treated with a solution of 5-methoxy-6-trifluoromethyl indoline (D11) (3.5 g, 16 mmoles) in dichloromethane (600 ml) and stirred overnight. The mixture was concentrated in vacuo and the residue triturated with diethyl ether. Filtration and washing with more diethyl ether gave the title compound (D26) (5.4 g, 81%).
後処理
- concentrationThe mixture was concentrated in vacuo
- customthe residue triturated with diethyl ether
- filtrationFiltration
- washwashing with more diethyl ether
出典と根拠
- ORDレコード
- ord-ea758860a31e454ba0a44fe7f2883def
- 出典データセット
- uspto-grants-1999_11
- 特許番号
- US05990133
反応ノート
読み込み中…