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

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.

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

ORDレコード

ord-809f861659cd41a7b0f787210052c141

出典データセット

uspto-grants-2003_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06610694B1