Formic Acid → Aldicarb sulfone

HRID 839865ノート

反応式

HRID 839865 の反応式
[CH:1](O)=O.[CH3:4][NH:5][C:6]([O:8][N:9]=[CH:10][C:11]([CH3:15])(SC)[CH3:12])=[O:7].OO.[S:18](=[O:22])(=O)(O)[OH:19]>C(Cl)Cl>[CH3:4][NH:5][C:6]([O:8][N:9]=[CH:10][C:11]([CH3:15])([S:18]([CH3:1])(=[O:22])=[O:19])[CH3:12])=[O:7]

参加物

6

反応物 4

HCID 284Formic AcidHCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 2086Aldicarb [ISO]

生成物 1

HCID 15438Aldicarb sulfone

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
40 °C

実験手順

15 grams of an 88 percent aqueous solution of formic acid was added to a mixture containing 30 grams of 2-methyl-2-(methylthio)propionaldehyde O-(methylcarbamoyl)oxime in 70 grams of methylene chloride solution. To the mixture was added 56 grams of a 30 percent aqueous hydrogen peroxide over a 15-20 minute period. During the course of addition, the reaction temperature rose from 25° to 40° C. with a gentle reflux of methylene chloride. After the addition of the peroxide solution, 6.0 grams of concentrated sulfuric acid was added dropwise at a rate to maintain the reflux at 40° C. When the addition was complete, the mixture was stirred for an additional 2.5 hours at 40.45° C. When the oxidation was over, 60-70 grams of the methylene chloride solvent was removed by evaporation under reduced pressure. The mixture was cooled to 5° C. and filtered. The solid reaction product was then washed with 25-30 grams of cold water and dried to constant weight. (2-Methyl-2-(Methylsulfonyl)propionaldehyde O-(methylcarbamoyl)oxime was obtained, m.p. 144°-145° C, having a 2-methyl-2-(methylsulfinyl)propionaldehyde O-(methylcarbamoyloxime (sulfide) content of less than 0.10 percent.

後処理

  1. additionDuring the course of addition
  2. customrose from 25° to 40° C.
  3. additionwas added dropwise at a rate
  4. temperatureto maintain the
  5. additionWhen the addition
  6. customwas removed by evaporation under reduced pressure
  7. temperatureThe mixture was cooled to 5° C.
  8. filtrationfiltered
  9. customThe solid reaction product
  10. washwas then washed with 25-30 grams of cold water
  11. customdried to constant weight

出典と根拠

ORDレコード
ord-31a0d5f10a07443dae3f7b285471f245
出典データセット
uspto-grants-1978_06
特許番号
US04097526

反応ノート

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