Diethyl (ethoxymethylene)malonate → 288251-62-7

HRID 2095807ノート

反応式

HRID 2095807 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 22228038288251-62-7収率 48.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-49e35ae4005d40fca09197084167709c
出典データセット
uspto-grants-2013_05
特許番号
US08445509B2

反応ノート

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