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

HRID 2231362

반응식

HRID 2231362 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d8b64bf095654dc39b5cf14e111a57a0
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04782156

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