Pyridine → alpha-Cyano-phenylacetic acid pentafluorophenyl ester

HRID 1980229

反応式

HRID 1980229 の反応式
[C:1]([CH:3]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:4]([OH:6])=[O:5])#[N:2].P(Cl)(Cl)(Cl)(Cl)Cl.[F:19][C:20]1[C:25](O)=[C:24]([F:27])[C:23]([F:28])=[C:22]([F:29])[C:21]=1[F:30].N1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl.ClCCl>[F:19][C:20]1[C:25]([O:5][C:4](=[O:6])[CH:3]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:1]#[N:2])=[C:24]([F:27])[C:23]([F:28])=[C:22]([F:29])[C:21]=1[F:30]

参加物

7

反応物 4

HCID 1049PyridineHCID 13041PentafluorophenolHCID 24819Phosphorus pentachlorideHCID 26403alpha-Cyanobenzeneacetic acid

生成物 1

HCID 20402416alpha-Cyano-phenylacetic acid pentafluorophenyl ester

試薬・触媒・溶媒 2

HCID 5943Carbon Tetrachloride溶媒HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

8 g. (0.05 moles) of α-cyano-phenylacetic acid are dissolved in 80 ml. of dichloromethane. 10.2 g. (0.05 moles) of phosphorus pentachloride are added and the mixture is stirred for two hours at the boiling point of dichloromethane. The solvent is distilled off and the residue is taken up in carbontetrachloride and the solution is added dropwise to 9.2 g. (0.05 moles) of pentafluorophenol and 4 ml. (0.05 moles) of pyridine-dissolved in 200 ml. of carbontetrachloride. The reaction mixture is cooled to 0° C. and the pyridine chlorohydrate is washed with 2n hydrochloride acid. The organic layer is washed twice with 40 ml. of water, dried over magnesium sulfate and evaporated. The α-cyano-phenylacetic acid-pentafluorophenyl ester is recrystallized from petrolether

後処理

  1. distillationThe solvent is distilled off
  2. additionthe solution is added dropwise to 9.2 g
  3. washthe pyridine chlorohydrate is washed with 2n hydrochloride acid
  4. washThe organic layer is washed twice with 40 ml
  5. dry with materialof water, dried over magnesium sulfate
  6. customevaporated
  7. customThe α-cyano-phenylacetic acid-pentafluorophenyl ester is recrystallized from petrolether

出典と根拠

ORDレコード
ord-b008978120024e89b3f15211d4f30f88
出典データセット
uspto-grants-1985_04
特許番号
US04508658

関連ノート

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