Chlorine → 3-Chloro-1-methyl-5-(pyrazin-2-yl)pyridin-2(1H)-one

HRID 1981513노트

반응식

HRID 1981513 반응식
[Cl:1]Cl.[CH3:3][N:4]1[CH:9]=[C:8]([C:10]2[CH:15]=[N:14][CH:13]=[CH:12][N:11]=2)[CH:7]=[CH:6][C:5]1=[O:16]>C(O)(=O)C>[Cl:1][C:6]1[C:5](=[O:16])[N:4]([CH3:3])[CH:9]=[C:8]([C:10]2[CH:15]=[N:14][CH:13]=[CH:12][N:11]=2)[CH:7]=1

참가 물질

4

반응물 2

HCID 24526Chlorine2회HCID 136450981-Methyl-5-(pyrazin-2-yl)pyridin-2(1H)-one

생성물 1

HCID 136451003-Chloro-1-methyl-5-(pyrazin-2-yl)pyridin-2(1H)-one

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

About 1.2 ml of condensed chlorine gas is introduced into a reaction mixture comprising 1-methyl-5-(2-pyrazinyl)-2-pyridone (3.2 g) dissolved in 200 ml of glacial acetic acid. After all the chlorine is added, stirring is stopped and the solid product filtered, washed with ether and air dried. The dried solid is suspended in distilled H2O to which saturated potassium carbonate is added until the pH is greater than 7. The resulting white solid is filtered, recrystallized from isopropanol, and NMR and IR indicate that it is the desired 3-chloro-1-methyl-5-(2-pyrazinyl)-2-pyridone compound, M.P. 197°-198° C.

후처리

  1. filtrationthe solid product filtered
  2. washwashed with ether and air
  3. customdried
  4. additionis added until the pH is greater than 7
  5. filtrationThe resulting white solid is filtered
  6. customrecrystallized from isopropanol, and NMR and IR

출처 및 근거

ORD 기록
ord-92c4ffb15a5b48918b98ee41222f868a
출처 데이터셋
uspto-grants-1986_06
특허 번호
US04593028

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