반응식
[N:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH:6]=1.[P:7]([O-:22])([O:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[O:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.N1CCCCC1P(=O)(O)O>>[NH:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH:6]1[P:7]([O:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:22])[O:8][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1참가 물질
반응 조건
- 온도
- 100 °C
실험 절차
This compound was prepared from the trimer of 2,3,4,5-tetrahydropyridine and diphenyl phosphite using the procedure previously described for the synthesis of the diethyl ester (Solodenko, V. A., Kukhar, V. P., Synthesis of DL-(2-Piperidyl) Phosphonic Acid, Zh. Obsh. Khim. 1987, 57, 2392). A mixture of the trimer (10 mmol, 2.5 g) and diphenyl phosphite (30 mmol, 7.0 g) was heated for 1.5 h at 100° C. under argon. The resulted crude diphenyl piperidine-2-phosphonate was dissolved in 100 mL of dry ether, undisolved material was removed by filtration, and the solution was saturated with gaseous HCl. The precipitated hydrochloride 2 was collected by filtration, washed with ether, dried and recrystallized from acetone to give a white solid in 41% yield: top. 172°-174° C.; 1H-NMR (D2O), δ (ppm) 1.5-2.4 (m, 6H), 3.05 (m, 1H), 3.45 (m, 1H), 4.10 (m, 1H), 6.9-7.4 (m, 10H); MS (FAB) m/e 318 (M-Cl)+. Anal. (C17H21NO3PCl): C, H, N, Cl.
출처 및 근거
- ORD 기록
- ord-16aa27e9e43240edb635a9e64316c6d0
- 출처 데이터셋
- uspto-grants-1996_08
- 특허 번호
- US05543396
연결된 노트
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