1-Boc-4-[(N-methoxy-N-methylcarbamoyl)methyl]piperidine → Tert-butyl 4-(2-oxopropyl)piperidine-1-carboxylate

HRID 1806183ノート

反応式

HRID 1806183 の反応式
[CH3:1][Mg]Cl.CON(C)[C:7](=[O:22])[CH2:8][CH:9]1[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]1>C1COCC1>[O:22]=[C:7]([CH3:1])[CH2:8][CH:9]1[CH2:10][CH2:11][N:12]([C:15]([O:17][C:18]([CH3:19])([CH3:20])[CH3:21])=[O:16])[CH2:13][CH2:14]1

参加物

4

反応物 2

HCID 229287811-Boc-4-[(N-methoxy-N-methylcarbamoyl)methyl]piperidineHCID 178418332HCID 178418332、化合物

生成物 1

HCID 12017169Tert-butyl 4-(2-oxopropyl)piperidine-1-carboxylate収率 99.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Added dropwise 3.0 M methylmagnesium chloride in THF (8.63 mL, 25.9 mmol) to a solution of tert-butyl 4-(2-(methoxy(methyl)amino)-2-oxoethyl)piperidine-1-carboxylate (5.93 g, 20.7 mmol) in THF (100 mL) at 0° C. Warmed to ambient temperature and stirred for 90 minutes. Partitioned between ether and 2N HCl, washed the organic layer twice with water, brine, dried, and concentrated to afford the title compound (4.95 g, 99.1% yield) as a clear oil.

後処理

  1. customPartitioned between ether and 2N HCl
  2. washwashed the organic layer twice with water, brine
  3. customdried
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-4b9f5d54ab234aae85caa55a30ecc721
出典データセット
uspto-grants-2013_01
特許番号
US08354540B2

反応ノート

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