Dimethyl Sulfoxide → HCID 9798400、化合物

HRID 1939924ノート

反応式

HRID 1939924 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([NH:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH2:21][CH2:22][C:23](=[O:26])[NH:24][N:25]=3)=[CH:16][CH:15]=2)=[O:8])[CH:2]=1.Br.C(O)(=O)C.CS(C)=O.C(OC(C)C)(C)C>C(O)(=O)C.C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([NH:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:21]=[CH:22][C:23](=[O:26])[NH:24][N:25]=3)=[CH:16][CH:15]=2)=[O:8])[CH:2]=1

参加物

7

反応物 4

HCID 679Dimethyl SulfoxideHCID 7914Diisopropyl EtherHCID 18977189HCID 18977189、化合物HCID 21893785Acetic Acid Mixture with Hydrobromic Acid

生成物 1

HCID 9798400HCID 9798400、化合物収率 89.5%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒

実験手順

In acetic acid (100 ml) was dissolved 10.0 g of 6-[4-(4-(pyridin-3-ylcarbonylamino)butyl)phenyl]-4,5-dihydropyridazin-3(2H)-one. 25 % hydrogen bromide-acetic acid (100 ml) was added to the solution, and the mixture was stirred at room temperature for 5 minutes. 2.9 g of dimethylsulfoxide was added to the mixture at room temperature, and the resulting mixture was stirred at the same temperature for 1 hour. Ethanol (150 ml) was added to the reaction mixture, and the mixture was stirred for 2 hours. Diisopropyl ether (150 ml) was further added to the mixture, and the resulting mixture was stirred for 2 hours. Precipitated crystal was collected by filtration, washed with diisopropyl ether and then dissolved in hydrated ethanol, and the solution was neutralized with aqueous ammonia. Precipitated crystal was collected by filtration, washed with water and then recrystallized from methanol to obtain 8.9 g of 6-[4-(4-(pyridin-3-ylcarbonylamino)butyl)phenyl]pyridazin-3(2H)-one.

後処理

  1. stirringthe resulting mixture was stirred at the same temperature for 1 hour
  2. stirringthe mixture was stirred for 2 hours
  3. stirringthe resulting mixture was stirred for 2 hours
  4. customPrecipitated crystal
  5. filtrationwas collected by filtration
  6. washwashed with diisopropyl ether
  7. dissolutiondissolved in hydrated ethanol
  8. customPrecipitated crystal
  9. filtrationwas collected by filtration
  10. washwashed with water
  11. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-f136f0bb397f4aee84d2f168eb94704f
出典データセット
uspto-grants-1997_12
特許番号
US05698554

反応ノート

読み込み中…