Water → HCID 1019799、化合物
反応式
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7](Cl)=[O:8].[Br:11][C:12]1[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=1[NH2:14].C(N(CC)CC)C.O>ClCCl>[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([NH:14][C:13]1[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=1[Br:11])=[O:8]参加物
6
実験手順
A mixture of 5-bromonicotinoyl chloride 5 (7.5 g, 33 mmol), 2-bromoaniline (5.86 g, 33 mmol) and triethylamine (14 mL, 100 mmol) in anhydrous dichloromethane (100 ml) was stirred under argon overnight. The resulting mixture was worked up with water and extracted with dichloromethane (200 mL×2). The organic phase was collected and dried over Na2SO4. After concentrated to 150 mL, white crystalline solid was crashed out. Filtration and washing with hexanes gave a white solid 6 (10.0 g, 85% yield).
後処理
- extractionextracted with dichloromethane (200 mL×2)
- customThe organic phase was collected
- dry with materialdried over Na2SO4
- concentrationAfter concentrated to 150 mL, white crystalline solid
- filtrationFiltration
- washwashing with hexanes
出典と根拠
- ORDレコード
- ord-0c0b2f5a5f6e4a59bb860e1af287adfe
- 出典データセット
- uspto-grants-2015_06
- 特許番号
- US09051284B2
反応ノート
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