Hydrochloric Acid → HCID 86690242, 화합물

HRID 80747노트

반응식

HRID 80747 반응식
[CH3:1][O:2][C@H:3]1[CH2:8][CH2:7][N:6](C(OC(C)(C)C)=O)[CH2:5][C:4]1([CH3:17])[CH3:16].[ClH:18].O1CCOCC1>CCOCC>[Cl-:18].[CH3:1][O:2][C@H:3]1[CH2:8][CH2:7][NH2+:6][CH2:5][C:4]1([CH3:17])[CH3:16]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 71244823(S)-tert-butyl 4-methoxy-3,3-dimethylpiperidine-1-carboxylate

생성물 1

HCID 86690242HCID 86690242, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To neat (S)-tert-butyl 4-methoxy-3,3-dimethylpiperidine-1-carboxylate (5.87 g, 24.1 mmol) was added 4.0 M HCl in dioxane (24.1 mL, 96.0 mmol), and the reaction mixture was stirred at room temperature for 16 h. Then, the reaction mixture was diluted with heptanes (60 mL) and Et2O (10 mL) and stirred at room temperature until a white solid crashed out. The heterogeneous mixture was then filtered and the white solid was collected to afford (S)-4-methoxy-3,3-dimethylpiperidin-1-ium chloride. 1H NMR (400 MHz, CDCl3) δ ppm 9.58 (br. s., 1 H), 9.23 (br. s., 1 H), 3.34 (s, 3 H), 3.09-3.24 (m, 2 H), 3.05 (t, J=10.0 Hz, 1 H), 2.97 (dd, J=5.4, 2.4 Hz, 1 H), 2.76 (d, J=13.1 Hz, 1 H), 2.04-2.17 (m, 1 H), 1.84-1.96 (m, 1 H), 1.19 (s, 3 H), 1.05 (s, 3 H).

후처리

  1. stirringstirred at room temperature until a white solid
  2. filtrationThe heterogeneous mixture was then filtered
  3. customthe white solid was collected

출처 및 근거

ORD 기록
ord-bd727c7f910a4b77a83605bae975cfd0
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846656B2

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