Ethyl formate → 2-(2,3-Dichlorophenyl)-3-oxo-propionitrile

HRID 234926

反応式

HRID 234926 の反応式
C[CH2:2][O-:3].[Na+].[Cl:5][C:6]1[C:11]([Cl:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:13][C:14]#[N:15].C(OCC)=O>C(O)C>[Cl:5][C:6]1[C:11]([Cl:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH:13]([CH:2]=[O:3])[C:14]#[N:15]

参加物

5

反応物 3

HCID 8025Ethyl formate2 回HCID 229020Benzeneacetonitrile, 2,3-dichloro-HCID 2723922Sodium ethoxide

生成物 1

HCID 197051252-(2,3-Dichlorophenyl)-3-oxo-propionitrile収率 45%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
80 °C

実験手順

To a solution of NaOEt (from 3.63 gms Na) in ethanol (500 ml) was added 2,3-dichlorophenylacetonitrile (Example 14.3) in ethanol (150 ml). Ethyl formate (16.67 gms) was then added and the mixture stirred at 80° C. for 45 minutes, before adding a further quantity of ethyl formate (2.78 gms). After stirring at 80° C. for a further 1.5 hours, the precipitate was filtered off and dried in vacuo. The solid was dissolved in water, filtered, acidified with concentrated hydrochloric acid and the precipitate filtered off and dried in vacuo, 14.35 gms, 45% yield.

後処理

  1. stirringAfter stirring at 80° C. for a further 1.5 hours
  2. filtrationthe precipitate was filtered off
  3. customdried in vacuo
  4. dissolutionThe solid was dissolved in water
  5. filtrationfiltered
  6. filtrationthe precipitate filtered off
  7. customdried in vacuo, 14.35 gms, 45% yield

出典と根拠

ORDレコード
ord-52fac0f666914fbd8c525fb4448e1779
出典データセット
uspto-grants-1997_01
特許番号
US05597827

関連ノート

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