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

HRID 637328

반응식

HRID 637328 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 1140Toluene용매

반응 조건

온도
36 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-3e2e03ce5751484982284f4156dbedf2
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04556674

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