5-Methyl-2-mercaptobenzothiazole synthesis
- Product Name:5-Methyl-2-mercaptobenzothiazole
- CAS Number:21303-50-4
- Molecular formula:C8H7NS2
- Molecular Weight:181.28
13194-69-9
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Yield:21303-50-4 73%
Reaction Conditions:
with iron(III) trifluoride;2,2'-bis-(diphenylphosphino)-1,1'-binaphthyl in N,N-dimethyl-formamide at 110; for 8 h;Inert atmosphere;Sealed tube;
Steps:
2. General experimental procedure
General procedure: A 25 mL reaction tube was charged with 2-haloaniline 1 (0.6 mmol), potassium o-ethyldithiocarbonate 2 (1.8 mmol), FeF3 (0.06 mmol), 2,2’-bis(diphenylphosphino)-1,1’-binaphthyl (0.03 mmol) and DMF (4 mL). The reaction vessel was flushed with argon for three times and sealed. Then the mixture was stirred electromagnetically in an oil bath at 110 for 3 - 21 hours. The reaction process was monitored by TLC on silica gel. After the reaction was completed, the reaction mixture was cooled to room temperature, then 4 mL HCl (3mol/L) was added and stirred for 30 minutes. Then the reaction mixture solution was extracted by ethyl acetate (3*20 mL). Subsequently, the combined organic solution were dried by anhydrous sodium sulfate and the target product was purified by silica gel colum chromatography (eluent: petroleum ether / ethylacetate) to give the corresponding pure product 3.
References:
Gao, Min;Lou, Chunqing;Zhu, Ning;Qin, Weijing;Suo, Quanling;Han, Limin;Hong, Hailong [Synthetic Communications,2015,vol. 45,# 20,p. 2378 - 2385] Location in patent:supporting information
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