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ChemicalBook CAS DataBase List 5-AMINO-3-METHYL-1,2,4-THIADIAZOLE

5-AMINO-3-METHYL-1,2,4-THIADIAZOLE synthesis

6synthesis methods
-

Yield:17467-35-5 32%

Reaction Conditions:

in methanol at 0 - 20; for 12 h;

Steps:

40.40-4

Compound LXII (5.1 g, 55 mmol) was dissolved in methanol (250 mL) and the resulting solution was cooled to 0° C. Potassium thiocyanate (5.3 g, 55 mmol) was then added. The resulting solution was stirred for 12 hours at room temperature, concentrated under reduced pressure, diluted with ethyl acetate (200 mL), and filtered under reduced pressure to remove a solid. The filtrate was concentrated under reduced pressure, creating a solid which was filtered under reduced pressure to yield Compound LXIII (2 g (32%)). The filtrate was further concentrated and applied to column chromatography (SiO2, n-hex:EA=4:1) to yield Compound LXIII (2 g (32%)).1H NMR (600 MHz, CD3OD) δ 3.27 (s, 3H)

References:

US2012/264727,2012,A1 Location in patent:Page/Page column 53

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