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

HRID 223183ノート

反応式

HRID 223183 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-968c1a452e6640f3abb1acc48271b301
出典データセット
uspto-grants-1982_10
特許番号
US04352815

反応ノート

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