HCID 13603776、化合物 → HCID 13519806、化合物
反応式
[O:1]=[C:2]1[CH2:11][CH2:10][C:9]2[C:4](=[C:5]([CH2:12][CH2:13][C:14]([OH:16])=O)[CH:6]=[CH:7][CH:8]=2)[NH:3]1>C(OC(=O)C)(=O)C>[CH2:10]1[C:9]2=[CH:8][CH:7]=[CH:6][C:5]3=[C:4]2[N:3]([C:14](=[O:16])[CH2:13][CH2:12]3)[C:2](=[O:1])[CH2:11]1参加物
3
反応条件
- 温度
- 100 °C
実験手順
1,2,3,4-Tetrahydro-2-oxo-8-quinolinepropanoic acid (2.1 g, 0.0096 mole) is dissolved in acetic anhydride (10 ml) and the solution is heated to 100° C. for one hour. Excess acetic anhydride is removed at reduced pressure and the residual anhydride is removed by addition of toluene and repeated concentration. The solid is recrystallized from ethyl acetate to yield pure 1,2,6,7-tetrahydro-3H,5H-benzo[ij]-quinolizine-3,5-dione, mp 136°-140° C.
後処理
- customExcess acetic anhydride is removed at reduced pressure
- customthe residual anhydride is removed by addition of toluene
- concentrationconcentration
- customThe solid is recrystallized from ethyl acetate
出典と根拠
- ORDレコード
- ord-dea381f0966749ccab4d86e2a94546a0
- 出典データセット
- uspto-grants-1986_04
- 特許番号
- US04582909
反応ノート
読み込み中…