Potassium Carbonate → 2-(3-Pyridyl)-3-(2,4-dichlorophenyl)-2-propenenitrile

HRID 1489156

반응식

HRID 1489156 반응식
[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[CH:4]=O.[N:11]1[CH:16]=[CH:15][CH:14]=[C:13]([CH2:17][C:18]#[N:19])[CH:12]=1.C([O-])([O-])=O.[K+].[K+]>C(O)=C>[N:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17](=[CH:4][C:3]2[CH:6]=[CH:7][C:8]([Cl:10])=[CH:9][C:2]=2[Cl:1])[C:18]#[N:19])[CH:12]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 134042,4-DichlorobenzaldehydeHCID 809233-Pyridineacetonitrile

생성물 1

HCID 542432932-(3-Pyridyl)-3-(2,4-dichlorophenyl)-2-propenenitrile수율 76%

시약·촉매·용매 1

HCID 11199Vinyl alcohol용매

실험 절차

To a stirred solution of 2,4-dichlorobenzaldehyde (5.0 g, 29 mmole) and 3-pyridylacetonitrile (3.05 ml, 29 mmole) in 150 ml absolute ethenol were added 3.95 g K2CO3. After stirring for about 15 minutes, a white solid precipitated out of the reaction mixture. The reaction mixture was stirred overnight and filtered. The filter cake was washed with absolute ethanol and dissolved in CH2Cl2. The CH2Cl2 solution was filtered and concentrated in vacuo. The resulting white solid was recrystallized from 3:2 hexane/ethyl acetate to give 6.0 g (76%) of the title compound.

후처리

  1. customa white solid precipitated out of the reaction mixture
  2. stirringThe reaction mixture was stirred overnight
  3. filtrationfiltered
  4. washThe filter cake was washed with absolute ethanol
  5. dissolutiondissolved in CH2Cl2
  6. filtrationThe CH2Cl2 solution was filtered
  7. concentrationconcentrated in vacuo
  8. customThe resulting white solid was recrystallized from 3:2 hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-ae26736518ad44dea01f8a8fc299cbd5
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677329

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