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

HRID 338765

反応式

HRID 338765 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 102624Ethyl 1-benzyl-4-oxopiperidine-3-carboxylate収率 92%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-23accd3ce0b947b5adda01e15ea94ba1
出典データセット
uspto-grants-2014_11
特許番号
US08889870B2

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