Benzoyl chloride → HCID 836063、化合物
反応式
[NH2:1][C:2]1[C:3]([Cl:8])=[N:4][CH:5]=[CH:6][CH:7]=1.[C:9](Cl)(=[O:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>N1C=CC=CC=1>[Cl:8][C:3]1[C:2]([NH:1][C:9](=[O:16])[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:7][CH:6]=[CH:5][N:4]=1参加物
4
実験手順
4.57 g 3-amino-2-chloropyridine (36 mmol) and 30 mL pyridine were mixed in an ice bath. 5.0 g benzoyl chloride (36 mol) was then added. After return to room temperature and reaction for 4 hr, the reaction was quenched by water. After extraction three times by ethyl acetate, an ethyl acetate layer was collected and washed by 1M HCl solution. After drying, filtration, concentration, and purification by silicon-gel column, 7.21 g solid was obtained, with a yield of 88%.
後処理
- customAfter return to room temperature and reaction for 4 hr
- customthe reaction was quenched by water
- extractionAfter extraction three times by ethyl acetate
- customan ethyl acetate layer was collected
- washwashed by 1M HCl solution
- customAfter drying
- filtrationfiltration, concentration, and purification by silicon-gel column
出典と根拠
- ORDレコード
- ord-ec26ed74f77e4255aa9122612271721d
- 出典データセット
- uspto-grants-2010_09
- 特許番号
- US07799918B2
反応ノート
読み込み中…