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

HRID 1632721노트

반응식

HRID 1632721 반응식
[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]

참가 물질

5

반응물 2

HCID 6497Dimethyl SulfateHCID 178468384CID 71354250

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6f9800a5172f431f972a01507faa2025
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04477448

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