HCID 18340730, 화합물 → Methyl 3-[(1,1-dimethylethoxy)carbonyl]-5-oxo-3-pyrrolidineacetate

HRID 1485092노트

반응식

HRID 1485092 반응식
[C:1]([C:3]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])([CH2:9][C:10](OC)=[O:11])[CH2:4][C:5]([O:7][CH3:8])=[O:6])#[N:2].[H][H]>CO.[Ni]>[CH3:8][O:7][C:5](=[O:6])[CH2:4][C:3]1([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:9][C:10](=[O:11])[NH:2][CH2:1]1

참가 물질

5

반응물 2

HCID 18340730HCID 18340730, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 18340822Methyl 3-[(1,1-dimethylethoxy)carbonyl]-5-oxo-3-pyrrolidineacetate수율 38.8%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

To a solution in methanol (70 mL) of the compound (5.00 g) obtained in step (1) above, a Raney nickel catalyst (about 7.5 g) was added. The mixture was stirred at 70° C. for 8 hours in a hydrogen atmosphere with 0.4 megapascals (MPa). After being cooled to room temperature, the reaction mixture was filtered through Celite (registered trademark) and the filtrate was concentrated under reduced pressure. To the resulting residue, diethyl ether (50 mL) and hexane (10 mL) were added and the mixture was stirred at room temperature for 15 minutes. The resulting precipitate was recovered by filtration to give tert-butyl 3-(2-methoxy-2-oxoethyl)-5-oxopyrrolidine-3-carboxylate as a colorless solid (1.75 g).

후처리

  1. filtrationthe reaction mixture was filtered through Celite (registered trademark)
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionTo the resulting residue, diethyl ether (50 mL) and hexane (10 mL) were added
  4. filtrationThe resulting precipitate was recovered by filtration

출처 및 근거

ORD 기록
ord-5c89d577111e4686bf53df92af974c38
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422240B2

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