Dimethyl Sulfate → 1-Methyl-4-phenylpyrrolidin-2-one

HRID 255911

反応式

HRID 255911 の反応式
[C:1]1([CH:7]2[CH2:11][NH:10][C:9](=[O:12])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(OC)(O[CH3:17])(=O)=O.[OH-].[Na+]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[CH3:17][N:10]1[CH2:11][CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:8][C:9]1=[O:12]

参加物

6

反応物 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 1213974-Phenyl-2-pyrrolidinone

生成物 1

HCID 124489631-Methyl-4-phenylpyrrolidin-2-one

試薬・触媒・溶媒 2

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 1140Toluene溶媒

反応条件

温度
36 °C

実験手順

A mixture of 4-phenyl-pyrrolidin-2-one (32.2 g; 0.2 mole), dimethyl sulfate (37.8 g; 0.3 mole), tetrabutyl ammonium hydrogensulfate (3.4 g; 0.01 mole), 50% aqueous sodium hydroxide solution (100 ml) and toluene (200 ml) is stirred at 36° C. for 5 hrs. After cooling, the aqueous phase is decanted, extracted with methylene chloride, and combined with the toluene phase. The organic phase is washed with water, dried and evaporated. The residue is distilled: b.p.0.2 mm Hg =120° C. Yield: 79%.

後処理

  1. temperatureAfter cooling
  2. customthe aqueous phase is decanted
  3. extractionextracted with methylene chloride
  4. washThe organic phase is washed with water
  5. customdried
  6. customevaporated
  7. distillationThe residue is distilled
  8. customb.p.0.2 mm Hg =120° C

出典と根拠

ORDレコード
ord-63d01324ad06414e9de36045f1c7651d
出典データセット
uspto-grants-1987_10
特許番号
US04699918

関連ノート

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