반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([CH3:13])([CH3:12])[CH:10]=O)=[CH:5][CH:4]=1.[C:14](Br)(Br)([Br:16])[Br:15].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>C(Cl)Cl>[CH3:12][C:9]([C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)([CH3:13])[CH:10]=[C:14]([Br:16])[Br:15]참가 물질
5
실험 절차
To a stirred solution of Compound 45 (3.0 g, 17 mmol) and CBr4 (11 g, 34 mmol) in CH2Cl2 (100 ml) was added PPh3 (18 g, 67 mmol) at r.t., and stirred for 1.5 h. The mixture was quenched by the addition of H2O, and extracted with CH2Cl2. The combined organic layers were washed with brine, dried over MgSO4, filtered, and concentrated. This was purified by SiO2 chromatography to give Compound 53 (2.5 g, 45%) as a colorless oil.
후처리
- customThe mixture was quenched by the addition of H2O
- extractionextracted with CH2Cl2
- washThe combined organic layers were washed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThis was purified by SiO2 chromatography
출처 및 근거
- ORD 기록
- ord-7fb77abeec4e4e33acaabbbc6f9447a3
- 출처 데이터셋
- uspto-grants-1998_08
- 특허 번호
- US05789423
연결된 노트
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