Cyanoacetic acid → Perfluorophenyl 2-cyanoacetate

HRID 1980225ノート

反応式

HRID 1980225 の反応式
[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]

参加物

5

反応物 3

HCID 9740Cyanoacetic acidHCID 10868DicyclohexylcarbodiimideHCID 13041Pentafluorophenol

生成物 1

HCID 20402415Perfluorophenyl 2-cyanoacetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0256dbc76ddc4550b62a98d4f7e406cb
出典データセット
uspto-grants-1985_04
特許番号
US04508658

反応ノート

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