Potassium Carbonate → HCID 18977189、化合物

HRID 2393747ノート

反応式

HRID 2393747 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 18977189HCID 18977189、化合物収率 80.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-495faf9748c74ec7987b6c654e6ed6f1
出典データセット
uspto-grants-1998_09
特許番号
US05808065

反応ノート

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