Acetic Anhydride → HCID 13345321、化合物
反応式
[CH3:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=O)[C:5]([C:11]([OH:13])=[O:12])=[CH:4][CH:3]=1.C(OC(=O)C)(=O)C>ClCCl>[CH3:1][C:2]1[N:7]=[C:6]2[C:8]([O:13][C:11](=[O:12])[C:5]2=[CH:4][CH:3]=1)=[O:10]参加物
4
反応条件
- 温度
- 110 °C
実験手順
A mixture of 6-methylpyridine-2,3-dicarboxylic acid (19.75 g) and acetic anhydride (51 ml) was stirred and heated in an oil bath (bath temperature 110° C.) for 5 hours. The solvent was removed in vacuo and a 2:1 mixture of dichloromethane and ether was added, giving a dark brown solid. A solution of this solid in dichloromethane was passed through a pad of silica gel, eluting with dichloromethane, and the solvent was then evaporated to give partially purified 6-methylpyridine-2,3-dicarboxylic acid anhydride (12.1 g).
後処理
- customThe solvent was removed in vacuo
- additiona 2:1 mixture of dichloromethane and ether
- additionwas added
- customgiving a dark brown solid
- washeluting with dichloromethane
- customthe solvent was then evaporated
出典と根拠
- ORDレコード
- ord-1f001ef2cea64ac6a0ed426e344da9d3
- 出典データセット
- uspto-grants-1999_08
- 特許番号
- US05935973
反応ノート
読み込み中…