Isopropanol → (9aR)-octahydropiperazino[2,1-c]morpholine
反応式
[CH2:1]1[C@H:6]2[CH2:7][NH:8][CH2:9][CH2:10][N:5]2[C:4](=O)[CH2:3][O:2]1.[H-].[H-].[H-].[H-].[Li+].[Al+3].CC(O)C.[O-]S([O-])(=O)=O.[Na+].[Na+]>O1CCOCC1>[CH2:1]1[C@H:6]2[CH2:7][NH:8][CH2:9][CH2:10][N:5]2[CH2:4][CH2:3][O:2]1参加物
6
実験手順
To a solution of (R)-hexahydro-pyrazino[2,1-c][1,4]oxazin-4-one (60 mg, 0.39 mmol) in dioxane (5 mL) was added LiAlH4 (1.5 mL, 1M solution in THF). The resulting mixture was heated at 80° C. for 2.5 h before the addition of iPrOH (0.5 mL) followed by a saturated aqueous solution of Na2SO4 (3 mL). Further Na2SO4 was added and the resulting mixture filtered through celite, washing with EtOAc. The resulting residue was purified by NH2 column to give the title compound as an oil (40 mg, 73%).
後処理
- filtrationthe resulting mixture filtered through celite
- washwashing with EtOAc
- customThe resulting residue was purified by NH2 column
出典と根拠
- ORDレコード
- ord-0de7cf8cbd134b419f5ede457cf48a8c
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08293735B2
反応ノート
読み込み中…