반응식
[CH2:1]1[CH:5]2[CH2:6][CH:7]([NH2:8])[CH:3]([CH2:4]2)[CH2:2]1.[CH3:9][CH:10]1[S:14](=[O:16])(=[O:15])[O:13][CH2:12][CH2:11]1>O1CCCC1>[CH:3]12[CH2:4][CH:5]([CH2:1][CH2:2]1)[CH2:6][CH:7]2[NH:8][CH2:12][CH2:11][CH:10]([S:14]([OH:16])(=[O:15])=[O:13])[CH3:9]참가 물질
4
실험 절차
To a solution of exo-2-aminonorbornane (1.0 g, 9.0 mmol) in tetrahydrofuran (THF, 10 mL) was added 2,4-butane sultone (1.28 g, 9.3 mmol). The solution was stirred at reflux for 3 hours. The reaction was cooled to room temperature. The solid was collected by filtration, washed with THF (2×20 mL) and dried in vacuo. 1H NMR (DMSO, 500 MHz) δ ppm 8.43 (s (broad), 1H), 2.96 (m, 3H), 2.62 (m, 1H), 2.38 (m, 1H), 2.28, (m, 1H), 1.91 (m, 1H), 1.82 (m, 1H), 1.61 (m, 1H), 1.54 (m, 2H), 1.42 (m, 2H), 1.12 (m, 6H). 13C (DMSO, 125 MHz) δ ppm 60.92, 60.79, 53.61, 53.21, 44.55, 44.36, 39.80, 39.55, 36.27, 36.15, 36.11, 35.98, 35.19, 35.13, 29.62, 29.43, 28.07, 26.88, 17.56, 14.11. ES-MS 248 (M+1).
후처리
- temperatureat reflux for 3 hours
- filtrationThe solid was collected by filtration
- washwashed with THF (2×20 mL)
- customdried in vacuo
출처 및 근거
- ORD 기록
- ord-45b730f9ad5b4cf39f54939210a94f65
- 출처 데이터셋
- uspto-grants-2014_02
- 특허 번호
- US08642801B2
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