Sulfuryl chloride → ethyl 3-chloro-2,4-dioxopentanoate
반응식
S(Cl)([Cl:4])(=O)=O.[O:6]=[C:7]([CH2:13][C:14](=[O:16])[CH3:15])[C:8]([O:10][CH2:11][CH3:12])=[O:9]>C(Cl)Cl>[Cl:4][CH:13]([C:14](=[O:16])[CH3:15])[C:7](=[O:6])[C:8]([O:10][CH2:11][CH3:12])=[O:9]참가 물질
4
실험 절차
A solution of sulfuryl chloride (7.08 g, 52 mmol) in 15 mL of CH2Cl2 was added dropwise to a solution of ethyl 2,4-dioxovalerate (7.91 g, 40 mmol) in 125 ml of CH2Cl2 at room temperature. After three hours TLC analysis indicated that all of the starting material had been consumed. The reaction mixture was washed with H2O (2×100 mL), dried over anhydrous MgSO4, filtered and concentrated in vacuo to give 7.84 g (81% yield) of the desired product as and orange oil: 1H NMR (CDCl3) δ14.4 (bs, 1H), 5.4 (s, 1H), 4.4-4.3 (m, 4H), 2.5 (s, 3H), 2.4 (s, 3H), 1.4-1.35 (s, 6H) for a 1:1 mixture of tautomers.
후처리
- customhad been consumed
- washThe reaction mixture was washed with H2O (2×100 mL)
- dry with materialdried over anhydrous MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-a0f1823b297c4cda8ba99cc18776b0b0
- 출처 데이터셋
- uspto-grants-2002_07
- 특허 번호
- US06413997B1
반응 노트
불러오는 중…