Ethanol → 5-(2-Ethoxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-7-pyrimidinone

HRID 862897

反応式

HRID 862897 の反応式
[CH2:1]([O:3][C:4]1[CH:24]=[CH:23][CH:22]=[CH:21][C:5]=1[C:6]([NH:8][C:9]1[C:10]([CH2:18][CH2:19][CH3:20])=[N:11][N:12]([CH3:17])[C:13]=1[C:14]([NH2:16])=[O:15])=O)[CH3:2].[OH-].[Na+].OO.C(O)C>O>[CH2:1]([O:3][C:4]1[CH:24]=[CH:23][CH:22]=[CH:21][C:5]=1[C:6]1[NH:16][C:14](=[O:15])[C:13]2[N:12]([CH3:17])[N:11]=[C:10]([CH2:18][CH2:19][CH3:20])[C:9]=2[N:8]=1)[CH3:2]

参加物

6

反応物 4

HCID 702EthanolHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 8501354-(2-Ethoxybenzamido)-1-methyl-3-propylpyrazole-5-carboxamide

生成物 1

HCID 1354014775-(2-Ethoxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-7-pyrimidinone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4-(2-Ethoxybenzamido)-1-methyl-3-n-propylpyrazole-5-carboxamide (223 g, 0.676 mol) was added portionwise to a solution of sodium hydroxide (54 g, 1.35 mol) and 30% hydrogen peroxide solution (224 ml) in water (2000 ml). Ethanol (700 ml) was added and the resulting mixture heated under reflux for 2.5 hours, cooled, then evaporated under vacuum. The resulting solid was treated with 2N hydrochloric acid (380 ml), with external cooling, and the mixture was extracted with dichloromethane (1×700 ml, 3×200 ml). The combined organic extracts were washed successively with saturated aqueous sodium carbonate solution (3×400 ml) and brine (300 ml), then dried (Na2SO4) and evaporated under vacuum.

後処理

  1. temperaturethe resulting mixture heated
  2. temperatureunder reflux for 2.5 hours
  3. temperaturecooled
  4. customevaporated under vacuum
  5. additionThe resulting solid was treated with 2N hydrochloric acid (380 ml), with external cooling
  6. extractionthe mixture was extracted with dichloromethane (1×700 ml, 3×200 ml)
  7. washThe combined organic extracts were washed successively with saturated aqueous sodium carbonate solution (3×400 ml) and brine (300 ml)
  8. dry with materialdried (Na2SO4)
  9. customevaporated under vacuum

出典と根拠

ORDレコード
ord-7a12599bfcb946318db19fd3111433b5
出典データセット
uspto-grants-1998_02
特許番号
US05719283

関連ノート

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