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

HRID 67321

反応式

HRID 67321 の反応式
[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

参加物

4

反応物 2

HCID 9032Potassium CyanideHCID 127597Ro 14-7437

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5900985991ac45158a44abf67892676c
出典データセット
uspto-grants-1982_08
特許番号
US04346030

関連ノート

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