Dimethyl methylphosphonate → Dimethyl (3-fluoro-2-oxoheptyl)phosphonate
反応式
[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]参加物
5
実験手順
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)
後処理
- additionwas added dropwise
- additionAfter addition
- stirringthe mixture was stirred at -78° C. for 45 minutes
- waitat room temperature for additional 45 minutes
出典と根拠
- ORDレコード
- ord-dc693c990ce24177ace9f8ec025d1025
- 出典データセット
- uspto-grants-1993_06
- 特許番号
- US05221763
反応ノート
読み込み中…