Methanol → HCID 577835、化合物

HRID 1885621ノート

反応式

HRID 1885621 の反応式
[C:1]1([CH3:16])[CH:6]=[CH:5][C:4]([N:7]2[C:11](=[O:12])[CH2:10][CH:9]([C:13]([OH:15])=[O:14])[CH2:8]2)=[CH:3][CH:2]=1.[CH3:17]O.S(=O)(=O)(O)O>C(Cl)Cl>[C:1]1([CH3:16])[CH:2]=[CH:3][C:4]([N:7]2[C:11](=[O:12])[CH2:10][CH:9]([C:13]([O:15][CH3:17])=[O:14])[CH2:8]2)=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 27418271-(4-Methylphenyl)-5-oxopyrrolidine-3-carboxylic acid

生成物 1

HCID 577835HCID 577835、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1-(4-Tolyl)-5-oxo-3-pyrrolidinecarboxylic acid (45.50 g) is suspended in methylene chloride (460 ml) and thereto are added methanol (50.5 ml) and conc. sulfuric acid (0.77 ml) and the mixture is refluxed for 19 hours. After cooling, the reaction mixture is concentrated under reduced pressure and the resulting residue is neutralized by adding water and aqueous sodium hydrogen carbonate solution thereto. The precipitated crystal is collected by filtration and washed with water to give the desired product (46.07 g), m.p. 71°-74° C.

後処理

  1. temperaturethe mixture is refluxed for 19 hours
  2. temperatureAfter cooling
  3. concentrationthe reaction mixture is concentrated under reduced pressure
  4. additionby adding water and aqueous sodium hydrogen carbonate solution
  5. filtrationThe precipitated crystal is collected by filtration
  6. washwashed with water

出典と根拠

ORDレコード
ord-efb1440428bc4feb972b93cda69fe5a1
出典データセット
uspto-grants-1992_09
特許番号
US05145865

反応ノート

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