Diethyl Ether → 3-(2,4-Dichlorophenyl)-3-oxopropanenitrile

HRID 981347

反応式

HRID 981347 の反応式
[Cl:1][C:2]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:3]=1[C:4]([O:6]CC)=O.[C:14](#[N:16])[CH3:15].[H-].[Na+].CCOCC>O1CCCC1>[Cl:1][C:2]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:3]=1[C:4]([CH2:15][C:14]#[N:16])=[O:6]

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 6342AcetonitrileHCID 24758Sodium hydrideHCID 42026Benzoic acid, 2,4-dichloro-, ethyl ester

生成物 1

HCID 136307283-(2,4-Dichlorophenyl)-3-oxopropanenitrile収率 28.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 43.8 g of ethyl 2,4-dichloro-benzoate and 8.2 g of anhydrous acetonitrile is added dropwise to a suspension of 6.1 g of 80% strength sodium hydride in 100 ml of anhydrous tetrahydrofuran in the course of about 1 hour under reflux. The mixture is heated at the boiling point under reflux for a further hour and cooled to room temperature and 150 ml of ether are added. The precipitate is filtered off with suction and dissolved in 50 ml of ice-water and the solution is acidified to pH=6 with 10% strength hydrochloric acid. The precipitate is filtered off cold with suction, rinsed with ice-water and dried in vacuo at 40° C. 12 g of 2,4-dichlorobenzoylacetonitrile of melting point 96°-98° C. are obtained.

後処理

  1. temperatureunder reflux
  2. temperatureThe mixture is heated at the boiling point
  3. temperatureunder reflux for a further hour
  4. filtrationThe precipitate is filtered off with suction
  5. dissolutiondissolved in 50 ml of ice-water
  6. filtrationThe precipitate is filtered off cold with suction
  7. washrinsed with ice-water
  8. customdried in vacuo at 40° C

出典と根拠

ORDレコード
ord-c61814e3bd0f4384bc3a0d027c4147fe
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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