Methyl chloroformate → Dimethyl 2-(2,4-difluorophenyl)piperidine-1,4-dicarboxylate

HRID 1963171노트

반응식

HRID 1963171 반응식
Cl.[F:2][C:3]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:4]=1[CH:10]1[CH2:15][CH:14]([C:16]([O:18][CH3:19])=[O:17])[CH2:13][CH2:12][NH:11]1.CCN(C(C)C)C(C)C.[C:29](Cl)(=[O:32])[O:30][CH3:31]>C(Cl)Cl>[F:2][C:3]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:4]=1[CH:10]1[CH2:15][CH:14]([C:16]([O:18][CH3:19])=[O:17])[CH2:13][CH2:12][N:11]1[C:29]([O:30][CH3:31])=[O:32]

참가 물질

5

반응물 3

HCID 6586Methyl chloroformateHCID 81531DiisopropylethylamineHCID 66731925Methyl 2-(2,4-difluorophenyl)piperidine-4-carboxylate hydrochloride

생성물 1

HCID 66734584Dimethyl 2-(2,4-difluorophenyl)piperidine-1,4-dicarboxylate수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Methyl 2-(2,4-difluorophenyl)piperidine-4-carboxylate hydrochloride (2.34 g, 8.02 mmol) was dissolved in DCM (50 mL), then DIPEA (3.50 mL, 20.05 mmol) was added. Methyl carbonochloridate (0.884 mL, 11.23 mmol) was added dropwise to the solution. The mixture was stirred at room temperature for 4 h, washed with 0.1 M HCl (100 mL) and satd NaHCO3 (100 mL), then dried through a phase-separator and evaporated yielding dimethyl 2-(2,4-difluorophenyl)piperidine-1,4-dicarboxylate (2.38 g, 95%) as an orange oil.

후처리

  1. washwashed with 0.1 M HCl (100 mL) and satd NaHCO3 (100 mL)
  2. customdried through a phase-separator
  3. customevaporated

출처 및 근거

ORD 기록
ord-64288e0017a94c4980df06aa7cc1d94f
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08415378B2

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