Diethyl Ether → (R)-4-(1-Aminoethyl)cyclohexan-1-ol
반응식
[OH:1][CH:2]1[CH2:7][CH2:6][CH:5]([C@H:8]([NH:10]C(=O)OC(C)(C)C)[CH3:9])[CH2:4][CH2:3]1.CCOCC>ClCCl>[NH2:10][C@@H:8]([CH:5]1[CH2:6][CH2:7][CH:2]([OH:1])[CH2:3][CH2:4]1)[CH3:9]참가 물질
4
실험 절차
Tert-butyl (R)-1-(4-hydroxycyclohexyl)ethylcarbamate (4.49 g, 18.45 mmol) was dissolved in dichloromethane (25 mL) and cooled to 0° C. under nitrogen. HCl 2M in Ether (27.68 mL of 2 M, 55.35 mmol) was added and the reaction allowed to warm slowly to ambient temperature for 18 hours. The reaction mixture was concentrated in vacuo. The crude mixture was dissolved in MeOH (25 mL). MP-Carbonate was added (11.75 g, 36.90 mmol) and the reaction mixture was stirred for 3 hours. The resin was filtered and the mother liquors were concentrated to dryness to afford the title compound as an off white solid (2.39 g, 90% yield).
후처리
- additionwas added
- concentrationThe reaction mixture was concentrated in vacuo
- dissolutionThe crude mixture was dissolved in MeOH (25 mL)
- additionMP-Carbonate was added (11.75 g, 36.90 mmol)
- filtrationThe resin was filtered
- concentrationthe mother liquors were concentrated to dryness
출처 및 근거
- ORD 기록
- ord-bc8d9b1309e74fb5a1f1c765ba87bee4
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08530489B2
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