참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | (Dimethyl sulfide)trihydroboron | HCID 12423031 | — |
| 반응물 | N,N-dipropyl-3,3-bis(diethoxyphosphinyl)propionamide | HCID 19689019 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Tetraethyl-3-(dipropylamino)-propane-1,1-bisphosphonate | HCID 53808940 | 60% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05728650 |
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| 출처 데이터셋 | uspto-grants-1998_03 |
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| ORD ID | ord-64a7cfe6196c4bb8ae1073b5f5bdac47 |
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| 출처 메모 | uspto-grants-1998_03 |
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