Water → 7-Phenyl-1,2-diazapin-3-one

HRID 2074

反応式

HRID 2074 の反応式
[C:1]([CH2:9][CH2:10][CH2:11][C:12]([OH:14])=O)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:16][NH2:17]>C1(C)C=CC=CC=1.CCOCC>[C:2]1([C:1]2[N:17]=[N:16][C:12](=[O:14])[CH:11]=[CH:10][CH:9]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 962WaterHCID 9321HydrazineHCID 73914delta-Oxobenzenepentanoic acid

生成物 1

HCID 856459747-Phenyl-1,2-diazapin-3-one収率 39%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒2 回HCID 3283Diethyl Ether溶媒

実験手順

To a mixture of 10 g (0.052 mole) of 4-benzoylbutyric acid in 300 ml of toluene, hydrazine was added in one portion and the reaction was heated to reflux until all water had ceased to azeotrope. The reaction mixture was cooled and the toluene was stripped off in vacuo. The residue was dissolved in 200 ml Et2O and washed with H2O (100 ml) and brine (100 ml). The ether extract was dried over anhydrous MgSO4, filtered and stripped to yield an orange semisolid which was triturated with ether to yield 3.8 g (39%) of the desired product as a yellow solid.

後処理

  1. additionwas added in one portion
  2. temperaturethe reaction was heated
  3. temperatureThe reaction mixture was cooled
  4. washwashed with H2O (100 ml) and brine (100 ml)
  5. extractionThe ether extract
  6. dry with materialwas dried over anhydrous MgSO4
  7. filtrationfiltered
  8. customto yield an orange semisolid which
  9. customwas triturated with ether

出典と根拠

ORDレコード
ord-e87aace35dd246b89ebaa26756e4c33e
出典データセット
uspto-grants-1998_03
特許番号
US05728694

関連ノート

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