Hydrochloric Acid → Cyclohexanone, 2-[(phenylmethoxy)methyl]-
反応式
[CH2:1]([O:8][CH2:9][CH:10]1[CH2:19][CH2:18][CH2:17][CH2:16][C:11]21OCC[O:12]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.C(=O)([O-])[O-].[Na+].[Na+]>CC(C)=O>[CH2:1]([O:8][CH2:9][CH:10]1[CH2:19][CH2:18][CH2:17][CH2:16][C:11]1=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
5
実験手順
A solution of 6-((Benzyloxy)methyl)-1,4-dioxaspiro[4.5]decane (2.4 g 9.1 mmol) in acetone (40 mL) was treated with 1.5N HCl (18 mL) and stirred at rt for 5 hours. The reaction mixture was neutralized with aqueous sodium carbonate and the volatile removed in vacuo. The residue was extracted with Et2O (3×50 mL) and the combined organic layer were washed with water (30 mL), brine (30 mL) and dried over sodium sulfate and concentrated to yield the desired product as pale yellow oil that was used in the next step without further purification. MS m/z 219.1 (M+1).
後処理
- customthe volatile removed in vacuo
- extractionThe residue was extracted with Et2O (3×50 mL)
- washthe combined organic layer were washed with water (30 mL), brine (30 mL)
- dry with materialdried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-5c7a327edd30448b824639d9178071f1
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09150568B2
反応ノート
読み込み中…