1,2-Oxathiolane, 3-methyl-, 2,2-dioxide → HCID 59771573, 화합물

HRID 239793

반응식

HRID 239793 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

  1. temperatureat reflux for 3 hours
  2. filtrationThe solid was collected by filtration
  3. washwashed with THF (2×20 mL)
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-45b730f9ad5b4cf39f54939210a94f65
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642801B2

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