Sodium → 3-(2,4-Dichloro-5-fluorophenyl)-3-oxopropanenitrile

HRID 981344

反応式

HRID 981344 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([F:9])=[CH:4][C:3]=1[C:10]1[O:14][N:13]=[CH:12][CH:11]=1.[Na]>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([F:9])=[CH:4][C:3]=1[C:10]([CH2:11][C:12]#[N:13])=[O:14]

参加物

4

反応物 2

HCID 5360545SodiumHCID 136307205-(2,4-Dichloro-5-fluorophenyl)-isoxazole

生成物 1

HCID 136307213-(2,4-Dichloro-5-fluorophenyl)-3-oxopropanenitrile収率 93.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

23.2 g (0.1 mole) of 5-(2,4-dichloro-5-fluoro- phenyl)-isoxazole are added in portions to a solution of 2.3 g (0.1 g atom) of sodium in 100 ml of absolute ethanol in the course of about 30 minutes while cooling with ice and stirring. The mixture is then stirred at room temperature for 1 hour, the alcohol is distilled off in vacuo, the residue is dissolved in about 1 liter of warm water, the solution is extracted twice with methylene chloride, the aqueous phase is acidified to pH=4 with 10 per cent strength hydrochloric acid (~38 ml) and the precipitate is filtered off cold with suction and dried in vacuo at 50° C. 21.7 g (93%) of 2,4-dichloro5-fluoro-benzoylacetonitrile of melting point 98°-99° C. are obtained.

後処理

  1. temperaturewhile cooling with ice
  2. stirringThe mixture is then stirred at room temperature for 1 hour
  3. distillationthe alcohol is distilled off in vacuo
  4. dissolutionthe residue is dissolved in about 1 liter of warm water
  5. extractionthe solution is extracted twice with methylene chloride
  6. filtrationthe precipitate is filtered off cold with suction
  7. customdried in vacuo at 50° C

出典と根拠

ORDレコード
ord-2d8b569c772d4cf39d97162ffd8acbc0
出典データセット
uspto-grants-1991_02
特許番号
US04990646

関連ノート

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