Potassium Carbonate → 3-(4-Fluorophenyl)-3-oxo-2-(4-pyridinyl)propanenitrile

HRID 1635922노트

반응식

HRID 1635922 반응식
[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][C:8]#[N:9])=[CH:3][CH:2]=1.[F:10][C:11]1[CH:26]=[CH:25][C:14]([C:15](ON2C(=O)CCC2=O)=[O:16])=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[F:10][C:11]1[CH:26]=[CH:25][C:14]([C:15](=[O:16])[CH:7]([C:4]2[CH:5]=[CH:6][N:1]=[CH:2][CH:3]=2)[C:8]#[N:9])=[CH:13][CH:12]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 41120852-(Pyridin-4-yl)acetonitrileHCID 10014374N-succinimidyl 4-fluorobenzoate

생성물 1

HCID 186256553-(4-Fluorophenyl)-3-oxo-2-(4-pyridinyl)propanenitrile수율 103%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

32 g of 4-pyridylacetonitrile and 86 g of 2,5-dioxo-pyrrolidinyl 4-fluorobenzoate were dissolved in 1.3 L of dimethylformamide. After the addition of 164 g of potassium carbonate, the resulting mixture was stirred at room temperature for a day. After the reaction mixture was filtered through cerite, the filtrate was concentrated under reduced pressure. After water was added to the residue, this solution was neutralized with an aqueous solution of hydrochloric acid. The precipitated crystals were collected by filtration, washed with diethyl ether, and then dried in a stream of air to obtain 67 g (103% yield) of the title compound.

후처리

  1. filtrationAfter the reaction mixture was filtered through cerite, the filtrate
  2. concentrationwas concentrated under reduced pressure
  3. additionAfter water was added to the residue
  4. filtrationThe precipitated crystals were collected by filtration
  5. washwashed with diethyl ether
  6. customdried in a stream of air

출처 및 근거

ORD 기록
ord-afd8a8dae8974d04a906caaa3f1f12c8
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06511997B1

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