Dichloromethane → 1-Benzyl 3-methyl 4-oxopiperidine-1,3-dicarboxylate

HRID 639851

반응식

HRID 639851 반응식
[O:1]=[C:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH:3]1[C:8]([O-:10])=[O:9].[CH2:11]([O:18][C:19](Cl)=[O:20])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[CH2:22](Cl)Cl>>[O:1]=[C:2]1[CH2:7][CH2:6][N:5]([C:19]([O:18][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:20])[CH2:4][CH:3]1[C:8]([O:10][CH3:22])=[O:9]

참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 10387Benzyl chloroformateHCID 179630544-Oxo-3-piperidinecarboxylate

생성물 1

HCID 157481361-Benzyl 3-methyl 4-oxopiperidine-1,3-dicarboxylate

실험 절차

To a stirred solution of 4-oxo-3-piperidinecarboxylate (5 g) in dry DCM (50 ml), under N2 atmosphere, TEA (9 mL) was added at rt and then, at 0° C., benzylchloroformate (4.2 mL) was added slowly and stirring was continued for 30 minutes at 0° C. and 1 h at RT. The mixture was quenched at 0° C. with HCl 2N. The aqueous phase was extracted with DCM (2 times) and the combined organic layers were washed with saturated NaCl aqueous solution, dried and concentrated in vacuo to give the title compound (7.5 g).

후처리

  1. customThe mixture was quenched at 0° C. with HCl 2N
  2. extractionThe aqueous phase was extracted with DCM (2 times)
  3. washthe combined organic layers were washed with saturated NaCl aqueous solution
  4. customdried
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3054fc7d726a43e89e8bd9c0ef608e4f
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691893B2

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