Ammonia → 3-Phenyl-6-pyridazone

HRID 877220

반응식

HRID 877220 반응식
[C:1]1([C:7](=O)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.[O:11]=[CH:12][C:13](O)=O.[NH3:16].O.[NH2:18]N>O>[C:1]1([C:7]2[CH:8]=[CH:13][C:12](=[O:11])[NH:16][N:18]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 7410AcetophenoneHCID 24654Hydrazine hydrate (1:1)HCID 15620607Glyoxylic acid, monohydrate

생성물 1

HCID 751063-Phenyl-6-pyridazone

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

19.6 g (162.95 mmol) of 1-phenylethanone and 5 g (54.32 mmol) of oxoacetate monohydrate were stirred at 100° C. for 2 hours. The reaction solution was then cooled to 40° C., and 20 ml of water and 4 ml of ammonia were added. The mixture was then twice extracted with 50 ml of dichloromethane. 2.64 ml (53.32 mmol) of hydrazine monohydrate were then added to the aqueous phase obtained, and the mixture was stirred at 100° C. for 2 hours. After the reaction, the reaction solution was cooled to room temperature. The precipitated crystals were filtered off with suction, washed with water and dried in a vacuum drying cabinet at 50° C. overnight. This gave 4.3 g (24.97 mmol, 15% of theory) of the title compound as colorless crystals.

후처리

  1. extractionThe mixture was then twice extracted with 50 ml of dichloromethane
  2. customobtained
  3. customAfter the reaction
  4. temperaturethe reaction solution was cooled to room temperature
  5. filtrationThe precipitated crystals were filtered off with suction
  6. washwashed with water
  7. customdried in a vacuum
  8. customdrying cabinet at 50° C. overnight

출처 및 근거

ORD 기록
ord-7abf0e199c0a420bbf6b4612125e53d1
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987256B2

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