Sulfuryl chloride → Methyl 2-chloro-3-oxo-3-(p-methoxyphenyl)propionate

HRID 1590544

반응식

HRID 1590544 반응식
[O:1]=[C:2]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1)[CH2:3][C:4]([O:6][CH3:7])=[O:5].S(Cl)([Cl:19])(=O)=O>ClC(Cl)(Cl)Cl>[Cl:19][CH:3]([C:2](=[O:1])[C:8]1[CH:9]=[CH:10][C:11]([O:14][CH3:15])=[CH:12][CH:13]=1)[C:4]([O:6][CH3:7])=[O:5]

참가 물질

4

반응물 2

HCID 24648Sulfuryl chlorideHCID 2759699Methyl 4-methoxy-beta-oxobenzenepropanoate

생성물 1

HCID 10014646Methyl 2-chloro-3-oxo-3-(p-methoxyphenyl)propionate수율 91.7%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

131 g of the methyl 3-oxo-3-(p-methoxyphenyl)propionate obtained in the above (1) was dissolved in 1.3 l of tetrachloromethane, and to the solution was added dropwise 85 g of sulfuryl chloride at 45° to 50° C. over 1 hour. After the dropwise addition, the mixture was stirred at the same temperature for 1 hour, cooled, washed with water and dried. Subsequently, the oily product of the residue obtained by evaporation of the solvent was distilled under reduced pressure to obtain 140 g of methyl 2-chloro-3-oxo-3-(p-methoxyphenyl)propionate.

후처리

  1. additionAfter the dropwise addition
  2. temperaturecooled
  3. washwashed with water
  4. customdried
  5. customSubsequently, the oily product of the residue obtained by evaporation of the solvent
  6. distillationwas distilled under reduced pressure

출처 및 근거

ORD 기록
ord-c9f670e3e219400c9f5c3831866b0c2e
출처 데이터셋
uspto-grants-1993_04
특허 번호
US05204248

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