Trifluoroacetic acid → HCID 178488964、化合物
反応式
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][C:3]=1[O:9][CH3:10].[F:11][C:12]([F:17])([F:16])[C:13](O)=O>>[CH3:10][O:9][C:3]1[C:2]2[NH:1][C:13]([C:12]([F:17])([F:16])[F:11])=[N:8][C:7]=2[CH:6]=[CH:5][CH:4]=1参加物
3
実験手順
A solution of 2,3-diaminoanisole (1.0 g) in trifluoroacetic acid (15 ml) was refluxed for 5 h and then stirred at room temperature overnight. Excess trifluoroacetic acid was removed in vacuo and the residue partitioned between ethyl acetate (50 ml) and water (50 ml). The organic phase was washed with saturated sodium bicarbonate solution (50 ml) and water (50 ml). Drying over anhydrous sodium sulfate and removal of the solvent in vacuo gave a brown residue. Purification by column chromatography eluting with 50% ethyl acetate in hexane gave the title compound as a yellow solid (1.4 g).
後処理
- customExcess trifluoroacetic acid was removed in vacuo
- customthe residue partitioned between ethyl acetate (50 ml) and water (50 ml)
- washThe organic phase was washed with saturated sodium bicarbonate solution (50 ml) and water (50 ml)
- dry with materialDrying over anhydrous sodium sulfate and removal of the solvent in vacuo
- customgave a brown residue
- customPurification by column chromatography
- washeluting with 50% ethyl acetate in hexane
出典と根拠
- ORDレコード
- ord-cd3646b14c6a4c6f81a7978aadde6c66
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06353010B1
反応ノート
読み込み中…