Acetyl chloride → HCID 12466147、化合物
反応式
[NH2:1][C:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][C:3]=1[C:11]#[N:12].[C:13](Cl)(=[O:15])[CH3:14]>N1C=CC=CC=1>[C:13]([NH:1][C:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][C:3]=1[C:11]#[N:12])(=[O:15])[CH3:14]参加物
4
実験手順
A solution of 3.86 g (0.024 mole) of 3-amino-2-benzofurancarbonitrile in 50 ml of pyridine is cooled in ice and treated over 15 minutes with 2.0 ml (2.21 g; 0.028 mole) of acetyl chloride. The mixture is stirred in ice an additional two hours and added to 250 g of ice/water. The precipitated crude product is filtered, washed with water, and recrystallized from aqueous methanol to yield 2.8 g (57% yield) of 3-(acetylamino)-2-benzofurancarbonitrile. A sample recrystallized a second time as above is analytically pure, mp 187°-189° C.
後処理
- customThe precipitated crude product
- filtrationis filtered
- washwashed with water
- customrecrystallized from aqueous methanol
出典と根拠
- ORDレコード
- ord-2ecdedc9eea7448da960dbf05264f4f4
- 出典データセット
- uspto-grants-1987_10
- 特許番号
- US04703053
反応ノート
読み込み中…