Dimethyl methylphosphonate → Dimethyl (3-fluoro-2-oxoheptyl)phosphonate
반응식
[CH3:1][P:2](=[O:7])([O:5][CH3:6])[O:3][CH3:4].C([Li])CCC.[F:13][CH:14]([CH2:19][CH2:20][CH2:21][CH3:22])[C:15](OC)=[O:16]>C1COCC1>[F:13][CH:14]([CH2:19][CH2:20][CH2:21][CH3:22])[C:15](=[O:16])[CH2:1][P:2](=[O:7])([O:5][CH3:6])[O:3][CH3:4]참가 물질
5
실험 절차
Dimethyl methylphosphonate (8.38 g) was dissolved in dry THF (250 ml) and cooled to -78° C. n-Butyllithium (1.6-M, 42 ml) was added dropwise, and the reaction was stirred for 10 minutes. The above methyl fluorocaproate (200 g) in THF (10 ml) was added dropwise. After addition, the mixture was stirred at -78° C. for 45 minutes, and then at room temperature for additional 45 minutes. The crude product obtained after the conventional work-up was chromatographed (hexane/ethyl acetate=1/1). Yield; 5.04 g (62 g)
후처리
- additionwas added dropwise
- additionAfter addition
- stirringthe mixture was stirred at -78° C. for 45 minutes
- waitat room temperature for additional 45 minutes
출처 및 근거
- ORD 기록
- ord-dc693c990ce24177ace9f8ec025d1025
- 출처 데이터셋
- uspto-grants-1993_06
- 특허 번호
- US05221763
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