Methanol → HCID 13772856、化合物

HRID 344229ノート

反応式

HRID 344229 の反応式
[C:1]1([C@@H:7]([N:9]2[C:13](=[O:14])[CH2:12][C@H:11]([C:15]([OH:17])=[O:16])[CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)O.[CH3:23]O>>[C:1]1([C@@H:7]([N:9]2[C:13](=[O:14])[CH2:12][C@H:11]([C:15]([O:17][CH3:23])=[O:16])[CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 723630(3S)-5-oxo-1-[(1S)-1-phenylethyl]pyrrolidine-3-carboxylic acid

生成物 1

HCID 13772856HCID 13772856、化合物

実験手順

(3S)-1-((S)-1-Phenylethyl)-5-oxo-3-pyrrolidinecarboxylic acid (666 g, optical purity not less than 99%) was dissolved in methanol (6 l), and conc. sulfuric acid (15 ml) was added at room temperature. The mixture was stirred at refluxing temperature for 7 hr. Methanol was evaporated, and the residue was extracted with ethyl acetate. The organic layer was washed with sodium hydrogencarbonate, dried over magnesium sulfate and concentrated under reduced pressure to give 738 g of methyl (3S)-1-((S)-1-phenylethyl)-5-oxo-3-pyrrolidine-carboxylate.

後処理

  1. temperatureat refluxing temperature for 7 hr
  2. customMethanol was evaporated
  3. extractionthe residue was extracted with ethyl acetate
  4. washThe organic layer was washed with sodium hydrogencarbonate
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-737d2879531445e9bf38f47de4c0651f
出典データセット
uspto-grants-1999_01
特許番号
US05864039

反応ノート

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