Potassium Cyanide → 2-Chloro-6-methylpyrimidine-4-carbonitrile

HRID 962382ノート

反応式

HRID 962382 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4]([CH3:9])[N:3]=1.[C-:10]#[N:11].[K+]>CC#N>[Cl:1][C:2]1[N:7]=[C:6]([C:10]#[N:11])[CH:5]=[C:4]([CH3:9])[N:3]=1

参加物

4

反応物 2

HCID 9032Potassium CyanideHCID 794712,4-Dichloro-6-methylpyrimidine

生成物 1

HCID 123550822-Chloro-6-methylpyrimidine-4-carbonitrile収率 24.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

24.5 g of 2,4-dichloro-6-methylpyrimidine and 9.8 g of potassium cyanide were dissolved in 150 ml of CH3CN and refluxed for 8 days. The solvent was evaporated, the residue was dissolved in 150 ml of ethyl acetate and extracted twice with 50 ml H2O. The organic layer was dried over Na2SO4, the solvent was evaporated and the residue was purified on silica gel using a 4:1 mixture of benzene and methyl tert.butyl ether as eluent to give 5.2 g (24.8%) of 2-chloro-4-cyano-6-methyl pyrimidine of m.p. 57° C.

後処理

  1. temperaturerefluxed for 8 days
  2. customThe solvent was evaporated
  3. dissolutionthe residue was dissolved in 150 ml of ethyl acetate
  4. extractionextracted twice with 50 ml H2O
  5. dry with materialThe organic layer was dried over Na2SO4
  6. customthe solvent was evaporated
  7. customthe residue was purified on silica gel using
  8. additiona 4:1 mixture of benzene and methyl tert.butyl ether as eluent

出典と根拠

ORDレコード
ord-8b0e0c5e2ef344649621ed9a43a25598
出典データセット
uspto-grants-1998_06
特許番号
US05759956

反応ノート

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