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

HRID 36898

반응식

HRID 36898 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 702Ethanol용매

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 ethanol 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 dissolve 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. dissolutiondissolve 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-5b8a828504824dbfaf9b32d9a5bbc2d0
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05418245

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