تفاعل #2350136

معادلة التفاعل

1-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine

triethylamine

6-isocyanato-1,4-benzodioxan

→

desired product

المردود 46.9%

N-(2,3-Dihydro-1,4-benzodioxin-6-yl)-4-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxamide

المردود 46.9%

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
2. 2
   أخرىThe residue was purified by high performance liquid chromatography (YMC HPLC Column
3. 3
   غسيلeluted with 10% to 100% Liquid A
4. 4
   أخرىLiquid B: an aqueous 0.1% trifluoroacetic acid solution) and recrystallized from a mixed solvent of hexane and tetrahydrofuran

الإجراء التجريبي

To a solution of 1-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine (200 mg, 0.812 mmol) and triethylamine (0.113 ml, 0.812 mmol) in tetrahydrofuran (2 ml) was added 6-isocyanato-1,4-benzodioxan (167 ml, 1.22 mmol) at room temperature, and the mixture was stirred at room temperature for 1 hour. The solvent was distilled off under reduced pressure. The residue was purified by high performance liquid chromatography (YMC HPLC Column eluted with 10% to 100% Liquid A; Liquid A: a 0.1% solution of trifluoroacetic acid in acetonitrile; Liquid B: an aqueous 0.1% trifluoroacetic acid solution) and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 161 mg (46.9%) of the desired product as a solid.

المصدر