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

HRID 1614078ノート

反応式

HRID 1614078 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 54521467Tert-butyl 2-methoxyimino-3-phenyliminobutyrate収率 64.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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 give tert-butyl 2-methoxyimino-3-phenyliminobutyrate (0.68 g).

後処理

  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

出典と根拠

ORDレコード
ord-27208230ae22427b919756e2c1ccecdc
出典データセット
uspto-grants-1993_03
特許番号
US05194432

反応ノート

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