Ethyl 1-benzyl-4-oxopiperidine-3-carboxylate hydrochloride → Ethyl 1-benzyl-4-oxopiperidine-3-carboxylate

HRID 338765

반응식

HRID 338765 반응식
Cl.[CH2:2]([N:9]1[CH2:14][CH2:13][C:12](=[O:15])[CH:11]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(=O)(O)[O-].[Na+]>ClCCl>[CH2:2]([N:9]1[CH2:14][CH2:13][C:12](=[O:15])[CH:11]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:10]1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 102623Ethyl 1-benzyl-4-oxopiperidine-3-carboxylate hydrochlorideHCID 516892Sodium Bicarbonate

생성물 1

HCID 102624Ethyl 1-benzyl-4-oxopiperidine-3-carboxylate수율 92%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In a 5 L 3-necked flask equipped with a mechanical stirrer and a dropping funnel was placed ethyl 1-benzyl-4-oxo-3-piperidinecarboxylate hydrochloride, (199.3 g, 0.67 mol) in dichloromethane (1.5 L). To this suspension was added saturated sodium bicarbonate (1.5 L) over one hour. After the solid dissolved, the organic layer was separated, washed with brine (250 mL), filtered through 1 PS filter paper and concentrated under reduced pressure to give 160.5 g (92%) of ethyl 1-benzyl-4-oxo-3-piperidinecarboxylate as an oil. NMR 60 MHz, (CDCl3), δ 7.3 (s, 5H), 4.2 (q, 2H), 3.6 (s, 2H), 2.3-3.6 (m, 6H), 1.3 (t, 3H).

후처리

  1. customIn a 5 L 3-necked flask equipped with a mechanical stirrer and a dropping funnel
  2. dissolutionAfter the solid dissolved
  3. customthe organic layer was separated
  4. washwashed with brine (250 mL)
  5. filtrationfiltered through 1 PS
  6. filtrationfilter paper
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-23accd3ce0b947b5adda01e15ea94ba1
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889870B2

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