Ammonia → Ethyl 5-methyl-8-nitro-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate

HRID 851643ノート

反応式

HRID 851643 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.N.[N+:23]([O-])([OH:25])=[O:24]>S(=O)(=O)(O)O>[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[C:11]([N+:23]([O-:25])=[O:24])[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

参加物

5

反応物 3

HCID 222AmmoniaHCID 944Nitric AcidHCID 127597Ro 14-7437

生成物 1

HCID 15480886Ethyl 5-methyl-8-nitro-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

2.85 g of ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate are dissolved in a mixture of 10 ml of 98 percent nitric acid and 15 ml of 98 percent sulphuric acid and heated to 120° for 2 hours. Subsequently, the mixture obtained is cooled to room temperature, poured onto ice, neutralized with about 25 percent ammonia and extracted with chloroform. The chloroform extracts are dried over magnesium sulphate and evaporated. After recrystallization of the residue from ethyl acetate, there is obtained ethyl 5,6-dihydro-5-methyl-8-nitro-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 197°-198°.

後処理

  1. temperatureheated to 120° for 2 hours
  2. customSubsequently, the mixture obtained
  3. additionpoured onto ice
  4. extractionextracted with chloroform
  5. dry with materialThe chloroform extracts are dried over magnesium sulphate
  6. customevaporated
  7. customAfter recrystallization of the residue from ethyl acetate

出典と根拠

ORDレコード
ord-d42eda0dde9647e195497ce89b5f6645
出典データセット
uspto-grants-1983_05
特許番号
US04386028

反応ノート

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