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

HRID 223183노트

반응식

HRID 223183 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.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

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 944Nitric AcidHCID 127597Ro 14-7437

생성물 1

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

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-968c1a452e6640f3abb1acc48271b301
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04352815

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