Water → 7-Phenyl-1,2-diazapin-3-one

HRID 2115

반응식

HRID 2115 반응식
[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

참가 물질

6

반응물 3

HCID 962WaterHCID 9321HydrazineHCID 73914delta-Oxobenzenepentanoic acid

생성물 1

HCID 856459747-Phenyl-1,2-diazapin-3-one수율 39%

시약·촉매·용매 2

HCID 1140Toluene용매2회HCID 3283Diethyl Ether용매

실험 절차

To a mixture of 10g (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.

후처리

  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

출처 및 근거

ORD 기록
ord-eff35b6820384eb2a5f2f60a585c840d
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728698

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