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

HRID 1632721ノート

反応式

HRID 1632721 の反応式
[C:1]([O:5][C:6](=[O:13])[C:7](=[N:11][OH:12])[C:8]([CH3:10])=[O:9])([CH3:4])([CH3:3])[CH3:2].S(OC)(O[CH3:18])(=O)=O>O.CO>[C:1]([O:5][C:6](=[O:13])[C:7](=[N:11][O:12][CH3:18])[C:8]([CH3:10])=[O:9])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 2

HCID 6497Dimethyl SulfateHCID 178468384CID 71354250

生成物 1

HCID 54110352Tert-butyl 2-methoxyimino-3-oxobutyrate

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 215 g of Na2CO2 in 2200 ml of water is added at room temperature a solution of 128 g of 2-hydroxyiminoacetoacetic acid-tert.butyl ester in 475 ml of methanol. 255 g of dimethyl sulphate are added, dropwise, at 8°-10°, and after 3 hours at 8°-10° and 15 hours at room temperature, the mixture is filtered. The filtrate is extracted 3 times with ethyl acetate extracted 3 times with ethyl acetate, dried over magnesium sulphate and evaporated to obtain the heading compound.

後処理

  1. filtration15 hours at room temperature, the mixture is filtered
  2. extractionThe filtrate is extracted 3 times with ethyl acetate
  3. extractionextracted 3 times with ethyl acetate
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. customto obtain the heading compound

出典と根拠

ORDレコード
ord-6f9800a5172f431f972a01507faa2025
出典データセット
uspto-grants-1984_10
特許番号
US04477448

反応ノート

読み込み中…