Benzenecarbothioamide, 4-(methylthio)- synthesis
- Product Name:Benzenecarbothioamide, 4-(methylthio)-
- CAS Number:53550-91-7
- Molecular formula:C8H9NS2
- Molecular Weight:183.29
21382-98-9
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Yield:53550-91-7 68%
Reaction Conditions:
with hydrogenchloride;O,O-Diethyl hydrogen phosphorodithioate in ethyl acetate at 20; for 22 h;
Steps:
3
4- (Methylthio) benzonitrile (12 g, 80.0 mmol) was dissolved in 4N hydrogen chloride in ethyl acetate (130 mL) , O,O-diethyl dithiophosphate (18.2 g, 88.0 mmol) was added, and the mixture was stirred at room temperature for 22 hours, Water (100 mL) was added to the reaction mixture and the mixture was extracted with ethyl acetate. The precipitated materials were filtered off and the filtrate was washed with saturated sodium chloride, dried, and concentrated. The residue was recrystallized from ethyl acetate to give the title compound (10 g, 54.5 mmol, yield 68%).IH-NMR (DMSO-d3) δ: 2.43 (s, 3H), 7.13 (s, 2H), 7.81 (m, 2H) , 8.32 (br s, 2H)
References:
WO2006/137658,2006,A1 Location in patent:Page/Page column 121
110-59-8
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105-56-6
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53550-91-7
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