Hydrochloric Acid → HCID 86690242、化合物

HRID 80747ノート

反応式

HRID 80747 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 86690242HCID 86690242、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-bd727c7f910a4b77a83605bae975cfd0
出典データセット
uspto-grants-2014_09
特許番号
US08846656B2

反応ノート

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