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

HRID 234926

반응식

HRID 234926 반응식
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]

참가 물질

5

반응물 3

HCID 8025Ethyl formate2회HCID 229020Benzeneacetonitrile, 2,3-dichloro-HCID 2723922Sodium ethoxide

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-52fac0f666914fbd8c525fb4448e1779
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05597827

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