반응 #169900

반응 방정식

N,N-diisopropylethylamine

4-amino-N-(3-bromo-4-fluorophenyl)-1,2,5-thiadiazole-3-carbothioamide

methyl trifluoromethanesulfonate

→

desired product

수율 98.0%

Methyl 4-amino-N-(3-bromo-4-fluorophenyl)-1,2,5-thiadiazole-3-carbimidothioate

수율 98.0%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   세척washed with water (50 mL) and brine (50 mL)
2. 2
   건조dried with sodium sulfate
3. 3
   여과filtered
4. 4
   농축concentrated

실험 절차

A solution of 4-amino-N-(3-bromo-4-fluorophenyl)-1,2,5-thiadiazole-3-carbothioamide (130 mg, 0.4 mmol) in dichloromethane (5.2 mL) was treated with methyl trifluoromethanesulfonate (64 μL, 0.6 mmol) followed by N,N-diisopropylethylamine (102 μL, 0.6 mmol) and stirred for 1 h. The reaction mixture was diluted with dichloromethane (100 mL), washed with water (50 mL) and brine (50 mL), dried with sodium sulfate, filtered, and concentrated to give the desired product (133 mg, 98%). LCMS for C10H9BrFN4S2 (M+H)+: m/z=346.8, 348.8.

출처