Formaldehyde → Dimethyl alpha-hydroxymethyl-alpha-fluoromalonate

HRID 258324

반응식

HRID 258324 반응식
[CH2:1]=[O:2].[F:3][CH:4]([C:9]([O:11][CH3:12])=[O:10])[C:5]([O:7][CH3:8])=[O:6]>C(=O)(O)[O-].[K+]>[OH:2][CH2:1][C:4]([F:3])([C:9]([O:11][CH3:12])=[O:10])[C:5]([O:7][CH3:8])=[O:6]

참가 물질

4

반응물 2

HCID 712FormaldehydeHCID 2737111Dimethyl fluoromalonate

생성물 1

HCID 10910147Dimethyl alpha-hydroxymethyl-alpha-fluoromalonate수율 90%

시약·촉매·용매 1

HCID 516893Potassium Bicarbonate촉매

실험 절차

48 g (0.48 mol) of potassium bicarbonate were dissolved in 535 g (6.59 mol) of aqueous formaldehyde solution (37% strength by weight) in a 4-liter glass flask. 841 g (5.6 mol) of dimethyl α-fluoromalonate were added dropwise to this solution., with stirring, in the course of 31/2 hours; the temperature was kept meanwhile within the range from 20° to 25° C. Stirring was continued for 2 hours at the same temperature, and during this time dimethyl α-hydroxymethyl-α-fluoromalonate was precipitated in the form of a colorless solid. 2,500 g of an aqueous, saturated solution of ammonium sulfate were then added to the reaction mixture, which was then extracted with methylene dichloride. The extraction solution was dried by means of anhydrous sodium sulfate. 906 g (90% of theory) of dimethyl a-hydroxymethyl-α-fluoromalonate were obtained after removing the methylene dichloride by distillation (bath temperature 40° C., 25 mbar).

후처리

  1. customwas kept meanwhile within the range from 20° to 25° C
  2. customduring this time dimethyl α-hydroxymethyl-α-fluoromalonate was precipitated in the form of a colorless solid
  3. addition2,500 g of an aqueous, saturated solution of ammonium sulfate were then added to the reaction mixture, which
  4. extractionwas then extracted with methylene dichloride
  5. dry with materialThe extraction solution was dried by means of anhydrous sodium sulfate

출처 및 근거

ORD 기록
ord-84d9a5d31aa4487e83177774f4556d5f
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05266668

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