Hydrochloric Acid → 4-Hydroxy-4-(4-iodophenyl)cyclohexanone
反応式
[I:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([OH:18])[CH2:17][CH2:16][C:11]3(OCC[O:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.Cl.[OH-].[Na+]>CC(C)=O>[OH:18][C:8]1([C:5]2[CH:4]=[CH:3][C:2]([I:1])=[CH:7][CH:6]=2)[CH2:9][CH2:10][C:11](=[O:12])[CH2:16][CH2:17]1参加物
5
実験手順
To a solution of 8-(4-iodo-phenyl)-1,4 dioxa-spiro[4.5]decan-8-ol (2 g) in acetone (10 mL) was added 5% HCl (20 mL) and the mixture was stirred at rt for 14 hours. The mixture was neutralized with 1N NaOH to pH 7, concentrated on rotvap, and then extracted with ethyl acetate (2×50 mL). The organic extracts were combined, washed with saline solution (2×50 mL), dried over sodium sulfate, concentrated in vacuo to provide 4-hydroxy-4-(4-iodophenyl)cyclohexanone (1.7 g, 98%). LCMS: 317.3 (M+H+, 100%).
後処理
- concentrationconcentrated on rotvap
- extractionextracted with ethyl acetate (2×50 mL)
- washwashed with saline solution (2×50 mL)
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-75037d548b4b41a1bf5302fff702f99d
- 出典データセット
- uspto-grants-2010_11
- 特許番号
- US07834021B2
反応ノート
読み込み中…