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Ammonia → HCID 54053191, 화합물

HRID 1378239
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HRID 1378239 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:12]=[N:13][C:14]([C:15](O)=[O:16])=[C:10]3[C@@H:9]3[CH2:18][CH2:19][N:8]3[C:7](=[O:20])[C:6]=2[CH:21]=1.C(N1C=CN=C1)([N:24]1C=CN=C1)=O.C(=O)=O.N>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:12]=[N:13][C:14]([C:15]([NH2:24])=[O:16])=[C:10]3[C@@H:9]3[CH2:18][CH2:19][N:8]3[C:7](=[O:20])[C:6]=2[CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 280Carbon DioxideHCID 682631,1'-CarbonyldiimidazoleHCID 54249109HCID 54249109, 화합물

생성물 1

HCID 54053191HCID 54053191, 화합물수율 92.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3.04 g (10.0 mmol) of (S)-7-chloro-12,12a-dihydro-9-oxo-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]benzodiazepine-1-carboxylic acid were suspended in 15 ml of N,N-dimethylformamide and treated portionwise at room temperature with 1.78 g (11.0 mmol) of 1,1'-carbonyldiimidazole. After the CO2 evolution had finished the clear brown solution was stirred at 50° for 30 min., cooled and treated dropwise at a temperature below 25° within about 10 min. with 2.5 ml of conc. ammonia. After stirring for 30 minutes the suspension obtained was evaporated and the residue was triturated with 30 ml of water. The white crystals were filtered off under suction and dried in a vacuum. There were obtained 2.8 g (92%) of (S)-7-chloro-12,12a-dihydro-9-oxo-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]benzodiazepine-1-carboxamide of m.p. 251°-253°.

후처리

  1. temperaturecooled
  2. stirringAfter stirring for 30 minutes the suspension
  3. customobtained
  4. customwas evaporated
  5. customthe residue was triturated with 30 ml of water
  6. filtrationThe white crystals were filtered off under suction
  7. customdried in a vacuum

출처 및 근거

ORD 기록
ord-97757a2519f0477f85f61789d4bb987b
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05665718

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