Potassium Carbonate → HCID 18977189, 화합물

HRID 1939923노트

반응식

HRID 1939923 반응식
C(=O)([O-])[O-].[K+].[K+].Cl.[C:8](Cl)(=[O:15])[C:9]1[CH:14]=[CH:13][CH:12]=[N:11][CH:10]=1.CN(C)C(=O)C.[NH2:23][CH2:24][CH2:25][CH2:26][CH2:27][C:28]1[CH:33]=[CH:32][C:31]([C:34]2[CH2:35][CH2:36][C:37](=[O:40])[NH:38][N:39]=2)=[CH:30][CH:29]=1>O>[N:11]1[CH:12]=[CH:13][CH:14]=[C:9]([C:8]([NH:23][CH2:24][CH2:25][CH2:26][CH2:27][C:28]2[CH:29]=[CH:30][C:31]([C:34]3[CH2:35][CH2:36][C:37](=[O:40])[NH:38][N:39]=3)=[CH:32][CH:33]=2)=[O:15])[CH:10]=1

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 31374DimethylacetamideHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 18977184HCID 18977184, 화합물

생성물 1

HCID 18977189HCID 18977189, 화합물수율 80.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

At an inner temperature of 0° C., 50 g of anhydrous potassium carbonate and then 8.5 g of nicotinic acid chloride hydrochloride were added to a N,N-dimethylacetamide suspension (270 ml) containing 9.0 g of 6-[4-(4-aminobutyl)phenyl]-4,5-dihydropyridazin-3(2H)-one. The reaction mixture was stirred at the same temperature for 30 minutes and then poured into 200 ml of ice water. After the mixture was stirred at room temperature for 2 hours, water (300 ml) was further added to the mixture, and precipitated crystal was collected by filtration. The resulting crystal was washed with water and then recrystallized from methanol to obtain 10.3 g of 6-[4-(4-(pyridin-3-ylcarbonylamino)butyl)phenyl]-4,5-dihydropyridazin-3(2H)-one.

후처리

  1. stirringAfter the mixture was stirred at room temperature for 2 hours
  2. customprecipitated crystal
  3. filtrationwas collected by filtration
  4. washThe resulting crystal was washed with water
  5. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-e67ebe5ecaaa4369938e83315f1a825c
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05698554

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