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

HRID 1590544

反応式

HRID 1590544 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c9f670e3e219400c9f5c3831866b0c2e
出典データセット
uspto-grants-1993_04
特許番号
US05204248

関連ノート

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