Potassium Cyanide → isopropyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine 3-carboxylate

HRID 67321

반응식

HRID 67321 반응식
[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:4]2[CH2:3]1.[C-:22]#N.[K+]>CC(O)C>[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][C:16]([C:17]([O:19][CH:20]([CH3:22])[CH3:21])=[O:18])=[C:4]2[CH2:3]1

참가 물질

4

반응물 2

HCID 9032Potassium CyanideHCID 127597Ro 14-7437

생성물 1

HCID 19735056isopropyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine 3-carboxylate

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

285 mg (1 mmol) of ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate and 50 mg of potassium cyanide are stirred at 60° C. for 72 hours in 10 ml of 2-propanol. Then, the mixture is concentrated on a rotary evaporator, the residue is partitioned between water and chloroform, extracted twice with chloroform, the chloroform phase is dried over magnesium sulphate and evaporated. There is obtained isopropyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine 3-carboxylate of melting point 190°-192° C. This product is uniform according to thin-layer chromatography.

후처리

  1. concentrationThen, the mixture is concentrated on a rotary evaporator
  2. customthe residue is partitioned between water and chloroform
  3. extractionextracted twice with chloroform
  4. dry with materialthe chloroform phase is dried over magnesium sulphate
  5. customevaporated

출처 및 근거

ORD 기록
ord-5900985991ac45158a44abf67892676c
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04346030

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