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 67627노트

반응식

HRID 67627 반응식
[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

참가 물질

4

반응물 2

HCID 9032Potassium CyanideHCID 22914412HCID 22914412, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ad746ad8df54458fb428af5bcb1ceb34
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04346036

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