5-METHYL-3-ISOXAZOLYL ISOTHIOCYANATE synthesis

Yield:321309-33-5 55.1%

Reaction Conditions:

with sodium carbonate in dichloromethane;water at 20; for 2.5 h;Cooling with ice;

Steps:

28 Synthesis of 3-isothiocyanato-5-methylisooxazole

3-amino-5-methylisooxazole (326 mg, 3.3 mmol) was dissolved in dichloromethane (6.5 mL), and ice-cooled. Thiophosgene (0.278 mL, 3.3x1.1 mmol) and sodium carbonate aqueous solution (769 mg, 3.3x2.2 mmol, 4 mL) were added, and stirred at room temperature for 2.5 hours. After the reaction, chloroform was added and washed with the saturated sodium chloride solution, dried with magnesium sulfate and the solvent was distilled off. The obtained residue was purified by Silica gel column chromatography (Biotage Isolera One, SANP 10 g, chloroform/methanol)to obtain title compound (yellow oil, 255 mg, 55.1%) .

References:

JP5829520,2015,B2 Location in patent:Paragraph 0405