Acetic Anhydride → 2-Acetylamino-6-chloroisonicotinic acid ethyl ester
反応式
[CH2:1]([O:3][C:4](=[O:13])[C:5]1[CH:10]=[C:9]([Cl:11])[N:8]=[C:7]([NH2:12])[CH:6]=1)[CH3:2].[C:14](OC(=O)C)(=[O:16])[CH3:15]>N1C=CC=CC=1.CN(C1C=CN=CC=1)C>[CH2:1]([O:3][C:4](=[O:13])[C:5]1[CH:10]=[C:9]([Cl:11])[N:8]=[C:7]([NH:12][C:14](=[O:16])[CH3:15])[CH:6]=1)[CH3:2]参加物
5
実験手順
A mixture of 14 g 2-amino-6-chloro-isonicotinic acid ethyl ester (Temple et al. J. Heterocycl. Chem. 1970, 7, 451) (70 mmol) in 150 ml acetic anhydride (large excess) and 150 ml pyridine (large excess) is stirred at 60° C. in the presence of 244 mg (2 mmol) DMAP for 16 h. The mixture is concentrated in vacuo, taken up in EtOAc and washed with 1N HCl, brine and 10% aq Na2CO3 to yield the title compound in the form of yellowish crystals (EtOH).
後処理
- concentrationThe mixture is concentrated in vacuo
- washwashed with 1N HCl, brine and 10% aq Na2CO3
出典と根拠
- ORDレコード
- ord-f9857cf0642b4e0194f39f5430c89e21
- 出典データセット
- uspto-grants-2011_10
- 特許番号
- US08039455B2
反応ノート
読み込み中…