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

HRID 911933노트

반응식

HRID 911933 반응식
[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

참가 물질

4

반응물 2

HCID 229287811-Boc-4-[(N-methoxy-N-methylcarbamoyl)methyl]piperidineHCID 178418332HCID 178418332, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-a5cbaa1e64124c1fa7c53e71dc986c62
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022223B2

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