Tetrahydrofuran → 7,7-Difluorooctahydropyrrolo[1,2-a]pyrazine
反応式
[F:1][C:2]1([F:13])[CH2:12][N:5]2[C:6](=O)[CH2:7][NH:8][C:9](=O)[C@@H:4]2[CH2:3]1.C1COCC1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>O>[F:13][C:2]1([F:1])[CH2:12][N:5]2[CH2:6][CH2:7][NH:8][CH2:9][CH:4]2[CH2:3]1参加物
6
反応条件
- 温度
- 0 °C
実験手順
A pressure bottle was charged with (S)-7,7-difluoro-hexahydropyrrolo[1,2-a]pyrazine-1,4-dione (350 mg, 1841 μmol) and THF under nitrogen, and the solution was cooled to 0° C. under nitrogen. Lithium aluminum hydride (3681 μl, 3681 μmol) was added, the mixture was allowed to warm to RT, followed by heating at reflux for 3 h. 2 mL of water was carefully added, followed by 2 mL of 6N NaOH. After stirring for 10 min, the mixture was filtered through Celite and washed with EtOAc. The filtrate was concentrated. GC/MS: [M+H]=163.
後処理
- temperatureto warm to RT
- temperatureby heating
- temperatureat reflux for 3 h
- filtrationthe mixture was filtered through Celite
- washwashed with EtOAc
- concentrationThe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-3fb2f9710315455eb5e83854e0570d07
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07981891B2
反応ノート
読み込み中…