Diethyl (ethoxymethylene)malonate → 288251-62-7

HRID 2095807노트

반응식

HRID 2095807 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][NH2:9])=[CH:4][CH:3]=1.Cl.C(=O)([O-])[O-].[K+].[K+].C([O:19][CH:20]=[C:21]([C:27](OCC)=O)[C:22]([O:24][CH2:25][CH3:26])=[O:23])C>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:20](=[O:19])[C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:27][NH:9]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6871Diethyl (ethoxymethylene)malonateHCID 11430Potassium CarbonateHCID 699814-Fluorophenylhydrazine hydrochloride

생성물 1

HCID 22228038288251-62-7수율 48.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a suspension of (4-fluorophenyl)hydrazine•hydrochloride (3 g, 18 mmol) and water (75 mL) were added potassium carbonate (5.6 g, 40 mmol) and diethyl ethoxymethylenemalonate (4.8 g, 22 mmol), and the mixture was heated under reflux for 7 hr. After cooling to room temperature, the mixture was washed with ethyl acetate. 6N Aqueous hydrochloric acid solution was added to the separated aqueous layer under ice-cooling. The precipitated solid was collected by filtration, washed with water and ethyl acetate/hexane (1/10), and dried under reduced pressure to give the title compound (2.2 g, 48%) as a yellow solid.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 7 hr
  3. washthe mixture was washed with ethyl acetate
  4. addition6N Aqueous hydrochloric acid solution was added to the separated aqueous layer under ice-
  5. temperaturecooling
  6. filtrationThe precipitated solid was collected by filtration
  7. washwashed with water and ethyl acetate/hexane (1/10)
  8. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-49e35ae4005d40fca09197084167709c
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445509B2

반응 노트

불러오는 중…