Potassium Cyanide → methyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a]thieno[2,3-f][1,4]diazepine-3-carboxylate

HRID 67478ノート

反応式

HRID 67478 の反応式
[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[S:10][CH:11]=[CH:12][C:6]=2[N:5]2[CH:13]=[N:14][C:15]([C:16]([O:18][CH2:19]C)=[O:17])=[C:4]2[CH2:3]1.[C-]#N.[K+]>CO>[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[S:10][CH:11]=[CH:12][C:6]=2[N:5]2[CH:13]=[N:14][C:15]([C:16]([O:18][CH3:19])=[O:17])=[C:4]2[CH2:3]1

参加物

4

反応物 2

HCID 9032Potassium CyanideHCID 22914412HCID 22914412、化合物

生成物 1

HCID 20515348methyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a]thieno[2,3-f][1,4]diazepine-3-carboxylate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A suspension of 430 mg (1.5 mmol) of ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a]thieno[2,3-f][1,4]-diazepine-3-carboxylate and 99 mg (1.5 mmol) of potassium cyanide in 15 ml of absolute methanol is heated under reflux for 3 hours while stirring. After evaporation in vacuo, the residue is treated with ca 20 ml of ice/water and extracted three times with ca 30 ml of chloroform each time. The combined chloroform phases are washed twice with ca 20 ml of water each time, dried over magnesium sulphate and evaporated. After washing with boiling ethyl acetate, there is obtained methyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a]thieno[2,3-f][1,4]diazepine-3-carboxylate of melting point 244°-245° C.

後処理

  1. temperatureis heated
  2. temperatureunder reflux for 3 hours
  3. customAfter evaporation in vacuo
  4. additionthe residue is treated with ca 20 ml of ice/water
  5. extractionextracted three times with ca 30 ml of chloroform each time
  6. washThe combined chloroform phases are washed twice with ca 20 ml of water each time
  7. dry with materialdried over magnesium sulphate
  8. customevaporated
  9. washAfter washing with boiling ethyl acetate

出典と根拠

ORDレコード
ord-ec3c28b9125b43bbb3219c637e2b8f09
出典データセット
uspto-grants-1982_08
特許番号
US04346034

反応ノート

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