Cyanoacetic acid → Perfluorophenyl 2-cyanoacetate

HRID 1980225노트

반응식

HRID 1980225 반응식
[C:1]([CH2:3][C:4]([OH:6])=[O:5])#[N:2].C1(N=C=NC2CCCCC2)CCCCC1.[F:22][C:23]1[C:28](O)=[C:27]([F:30])[C:26]([F:31])=[C:25]([F:32])[C:24]=1[F:33]>ClCCl>[F:22][C:23]1[C:28]([O:5][C:4](=[O:6])[CH2:3][C:1]#[N:2])=[C:27]([F:30])[C:26]([F:31])=[C:25]([F:32])[C:24]=1[F:33]

참가 물질

5

반응물 3

HCID 9740Cyanoacetic acidHCID 10868DicyclohexylcarbodiimideHCID 13041Pentafluorophenol

생성물 1

HCID 20402415Perfluorophenyl 2-cyanoacetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

4.25 g. (0.05 moles) of cyanoacetic acid are dissolved in 100 ml. of dichloromethane and a solution of 10.3 g. (0.05 moles) of dicyclohexylcarbodiimide and 9.2 g. (0.05 moles) of pentafluorophenol in 50 ml. of dichloromethane is added. The mixture is stirred at room temperature for 4 hours, cooled to 0° C. and the precipitated dicyclohecylcarbodiimide is removed by filtration, the solvent is removed by distillation and the residue is taken up in petrolether and the precipitated ester is filtered, trituated with petrolether, washed and dried.

후처리

  1. temperaturecooled to 0° C.
  2. customthe precipitated dicyclohecylcarbodiimide is removed by filtration
  3. customthe solvent is removed by distillation
  4. filtrationthe precipitated ester is filtered
  5. washwashed
  6. customdried

출처 및 근거

ORD 기록
ord-0256dbc76ddc4550b62a98d4f7e406cb
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04508658

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