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

HRID 751652노트

반응식

HRID 751652 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 220613544-(2-Methoxyethoxy)piperidine hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-f467755a87d641e888388f4890f434f6
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07405210B2

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