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

HRID 1485092ノート

反応式

HRID 1485092 の反応式
[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

参加物

5

反応物 2

HCID 18340730HCID 18340730、化合物HCID 178418361HCID 178418361、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-5c89d577111e4686bf53df92af974c38
出典データセット
uspto-grants-2016_08
特許番号
US09422240B2

反応ノート

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