Dimethyl Sulfate → Tert-butyl 2-methoxyimino-3-phenyliminobutyrate

HRID 1088051노트

반응식

HRID 1088051 반응식
[OH:1][N:2]=[C:3]([C:11](=[N:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH3:12])[C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5].[C:20](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>CC(C)=O>[CH3:20][O:1][N:2]=[C:3]([C:11](=[N:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[CH3:12])[C:4]([O:6][C:7]([CH3:10])([CH3:8])[CH3:9])=[O:5]

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 136404523Tert-butyl 2-hydroxyimino-3-phenyliminobutyrate

생성물 1

HCID 54521467Tert-butyl 2-methoxyimino-3-phenyliminobutyrate수율 64.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of tert-butyl 2-hydroxyimino-3-phenyliminobutyrate (1.0 g) in acetone (10 ml) was added potassium carbonate (0.63 g) and dimethyl sulfate (0.43 ml) under ice-cooling. The mixture was stirred at the same temperature for 30 minutes and stirred at ambient temperature for 4 hours. The resulting suspension was poured into ice-water and extracted with diisopropyl ether. The organic layer was washed with water, dried over magnesium sulfate, and evaporated in vacuo. The residual oil was subjected to column chromatography on silica gel to give tert-butyl 2-methoxyimino-3-phenyliminobutyrate (0.68 g).

후처리

  1. temperaturecooling
  2. stirringstirred at ambient temperature for 4 hours
  3. extractionextracted with diisopropyl ether
  4. washThe organic layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-3dbc91e6092e4308863622c1f28fe6ca
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960766

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