Hydrochloric Acid → 4-Hydroxy-4-(4-iodophenyl)cyclohexanone
반응식
[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]1참가 물질
5
실험 절차
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%).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-77d62ad472e74c47ac5286b7391abdb5
- 출처 데이터셋
- uspto-grants-2014_05
- 특허 번호
- US08729063B2
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