반응식
[CH2:1]([N:4]([CH2:25][CH2:26][CH3:27])[C:5](=O)[CH2:6][CH:7]([P:16]([O:21][CH2:22][CH3:23])([O:18][CH2:19][CH3:20])=[O:17])[P:8]([O:13][CH2:14][CH3:15])([O:10][CH2:11][CH3:12])=[O:9])[CH2:2][CH3:3].B.CSC.Cl>C1COCC1>[CH2:19]([O:18][P:16]([CH:7]([P:8]([O:10][CH2:11][CH3:12])(=[O:9])[O:13][CH2:14][CH3:15])[CH2:6][CH2:5][N:4]([CH2:1][CH2:2][CH3:3])[CH2:25][CH2:26][CH3:27])(=[O:17])[O:21][CH2:22][CH3:23])[CH3:20]참가 물질
반응 조건
- 온도
- 0 °C
실험 절차
A solution of N,N-dipropyl-3,3-bis(diethoxyphosphinyl)propionamide (1.25 g, 2.9 mmol) in THF (7.1 ml) was cooled to 0° C., and borane-methylsulfide (0.71 ml, 7.1 mmol) was added via syringe. The reaction was stirred at 0° C. for 20 minutes, then warmed at 65 C. for 3 hours. The reaction mixture was cooled to 0° C. and 6N HCl (6 ml) was added carefully. The solvent was removed m vacuo, and the residue was treated with methanol (5 ml) and concentrated. The residue was dissolved in water (10 ml) and extracted with Et2O (3×10 ml). The aqueous layer was made basic to phenolphthalein with solid KOH and saturated with NaCl. The product was extracted into dichloromethane (5×20 ml), dried (Na2SO4) and concentrated to give the title compound (0.71 g, 60%).
후처리
- temperaturewarmed at 65 C
- waitfor 3 hours
- temperatureThe reaction mixture was cooled to 0° C.
- customThe solvent was removed m vacuo
- additionthe residue was treated with methanol (5 ml)
- concentrationconcentrated
- dissolutionThe residue was dissolved in water (10 ml)
- extractionextracted with Et2O (3×10 ml)
- extractionThe product was extracted into dichloromethane (5×20 ml)
- dry with materialdried (Na2SO4)
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-64a7cfe6196c4bb8ae1073b5f5bdac47
- 출처 데이터셋
- uspto-grants-1998_03
- 특허 번호
- US05728650
연결된 노트
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