Potassium Hydroxide → 3',4'-dihydro-2-oxospiro[piperidine-4,4'(1H)-quinoline]
反応式
F[C:2](F)(F)[C:3]([NH2:5])=[O:4].[NH:8]1[CH2:13][CH2:12][C:11]2([C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)C(=O)C2)[CH2:10][CH2:9]1.[OH-].[K+]>CO.O>[O:4]=[C:3]1[CH2:2][C:11]2([C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[NH:8][CH2:9][CH2:10]2)[CH2:12][CH2:13][NH:5]1参加物
4
実験手順
A solution of 49 mg (0.157 mmol) of the high RF material from Step B in methanol/water 4:1 with excess potassium hydroxide was stirred over night. The solution was concentrated and water and ethyl acetate were added to the residue. The layers were separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate and concentrated to give 31 mg (0.143 mmol) of the title compound.
後処理
- concentrationThe solution was concentrated
- additionwater and ethyl acetate were added to the residue
- customThe layers were separated
- extractionthe aqueous layer was extracted with ethyl acetate
- dry with materialThe combined organic layers were dried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-2bd4a4afe0854aea8e7bb6d120c912d0
- 出典データセット
- uspto-grants-1997_07
- 特許番号
- US05652235
反応ノート
読み込み中…