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

HRID 639851

反応式

HRID 639851 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3054fc7d726a43e89e8bd9c0ef608e4f
出典データセット
uspto-grants-2010_04
特許番号
US07691893B2

関連ノート

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