Hydrochloric Acid → 4-(2-Methoxyethoxy)piperidine hydrochloride

HRID 1693397ノート

反応式

HRID 1693397 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([O:14][CH2:15][CH2:16][O:17][CH3:18])[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:19].O1CCOCC1>CO>[ClH:19].[CH3:18][O:17][CH2:16][CH2:15][O:14][CH:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 57476927Tert-butyl 4-(2-methoxyethoxy)piperidin-1-carboxylate

生成物 1

HCID 220613544-(2-Methoxyethoxy)piperidine hydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 4-(2-methoxyethoxy)-piperidine-1-carboxylic acid tert-butyl ester (Preparation 81, 114 mg, 0.44 mmol) in methanol (3 mL) was added 4M HCl in dioxane (550 μL, 2.20 mmol) and the reaction stirred at rt for 16 h. Solvent was removed in vacuo and the crude residue dissolved in water (10 mL). The aqueous solution was extracted with ethyl acetate (2×10 mL) then concentrated in vacuo. Purification by trituration in ethyl acetate gave the title compound as the hydrochloride salt. δH (CD3OD): 3.74-3.67 (1H, m), 3.64 (2H, m), 3.56 (2H, m), 3.40-2.39 (7H, m), 2.11-1.96 (2H, m), 1.93-1.83 (2H, m).

後処理

  1. customSolvent was removed in vacuo
  2. dissolutionthe crude residue dissolved in water (10 mL)
  3. extractionThe aqueous solution was extracted with ethyl acetate (2×10 mL)
  4. concentrationthen concentrated in vacuo
  5. customPurification by trituration in ethyl acetate

出典と根拠

ORDレコード
ord-0e15bd9866244e47911e59b9e21eefac
出典データセット
uspto-grants-2012_04
特許番号
US08158622B2

反応ノート

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