Methyl iodide → 6-chloro-2-methyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one

HRID 397572노트

반응식

HRID 397572 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[NH:9][N:10]=2)[N:7]=1.[C:12](=O)([O-])[O-].[K+].[K+].CI>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[N:9]([CH3:12])[N:10]=2)[N:7]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 64071826-chloro-2H,3H-[1,2,4]triazolo[4,3-b]pyridazin-3-one

생성물 1

HCID 230003286-chloro-2-methyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one수율 67.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

0.853 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one was dissolved in 5 ml of N,N-dimethylformamide; 0.83 g of potassium carbonate was added; with stirring at room temperature, 0.5 ml of methyl iodide was added. After stirring at room temperature for 15 hours, ice water and saline were added; the reaction mixture was extracted with ethyl acetate-tetrahydrofuran (1:1); the extract was washed with saline and dried over magnesium sulfate. After concentration under reduced pressure, the crystal obtained was collected by filtration, washed with diethyl ether, and dried, to yield 0.62 g of the title compound.

후처리

  1. stirringAfter stirring at room temperature for 15 hours
  2. extractionthe reaction mixture was extracted with ethyl acetate-tetrahydrofuran (1:1)
  3. washthe extract was washed with saline
  4. dry with materialdried over magnesium sulfate
  5. concentrationAfter concentration under reduced pressure
  6. customthe crystal obtained
  7. filtrationwas collected by filtration
  8. washwashed with diethyl ether
  9. customdried

출처 및 근거

ORD 기록
ord-809f861659cd41a7b0f787210052c141
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610694B1

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