Hydrochloric Acid → 3a-Methyl-6-(3-oxo-butyl)-1,2,4,5,9a,9b-hexahydro-3aH-9-oxa-cyclopenta[a]naphthalene-3,7-dione
反応式
Cl.[CH3:2][C:3]12[C:24](=[O:25])[CH2:23][CH2:22][CH:4]1[CH:5]1[C:10]([CH2:11][CH2:12]2)=[C:9]([CH2:13][CH2:14][C:15]2([CH3:20])OCC[O:16]2)[C:8](=[O:21])[CH2:7][O:6]1>CC(C)=O>[CH3:2][C:3]12[C:24](=[O:25])[CH2:23][CH2:22][CH:4]1[CH:5]1[C:10]([CH2:11][CH2:12]2)=[C:9]([CH2:13][CH2:14][C:15](=[O:16])[CH3:20])[C:8](=[O:21])[CH2:7][O:6]1参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
3 N Hydrochloric acid (0.85 mL) was added to a stirred solution of the crude 3a-Methyl-6-[2-(2-methyl-[1,3]dioxolan-2-yl)-ethyl]-1,2,4,5,9a,9b-hexahydro-3aH-9-oxa-cyclopenta[a]naphthalene-3,7-dione in acetone (50 mL) at room temperature. The reaction mixture was stirred at room temperature for 0.5 h. The reaction was quenched with saturated sodium bicarbonate aqueous solution (50 mL), and then the acetone was removed under reduced pressure. The residue was diluted with brine (50 mL), extracted with ethyl acetate (2×100 mL), and the combined organic layer was dried with magnesium sulfate. The resulting solution was filtered and the solvent evaporated to yield an oil, which was used in subsequent steps without further purification.
後処理
- customThe reaction was quenched with saturated sodium bicarbonate aqueous solution (50 mL)
- customthe acetone was removed under reduced pressure
- additionThe residue was diluted with brine (50 mL)
- extractionextracted with ethyl acetate (2×100 mL)
- dry with materialthe combined organic layer was dried with magnesium sulfate
- filtrationThe resulting solution was filtered
- customthe solvent evaporated
- customto yield an oil, which
- customwas used in subsequent steps without further purification
出典と根拠
- ORDレコード
- ord-6a217ed4844040039b0fa7fccc495abc
- 出典データセット
- uspto-grants-2010_07
- 特許番号
- US07763648B2
反応ノート
読み込み中…