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ChemicalBook CAS DataBase List 6-Benzothiazolecarbonitrile,2,3-dihydro-2-thioxo-(9CI)
315228-79-6

6-Benzothiazolecarbonitrile,2,3-dihydro-2-thioxo-(9CI) synthesis

7synthesis methods
Potassium ethylxanthate

140-89-6

4-AMINO-2-IODOBENZONITRILE  98

33348-34-4

6-Benzothiazolecarbonitrile,2,3-dihydro-2-thioxo-(9CI)

315228-79-6

The general procedure for the synthesis of 2-mercaptobenzothiazole-6-carbonitrile from potassium ethylxanthate and 4-amino-3-iodobenzonitrile was as follows: 4-amino-3-iodobenzonitrile (0.6 mmol), potassium ethylxanthate (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 replaced three times with argon and sealed. Subsequently, the mixture was placed in an oil bath at 110 °C and the reaction was electromagnetically stirred for 3-21 hours. The reaction process was monitored by silica gel thin layer chromatography (TLC). After completion of the reaction, the reaction mixture was cooled to room temperature, 4 mL of 3 mol/L hydrochloric acid solution was added and stirred for 30 min. The reaction mixture was extracted with ethyl acetate (3 x 20 mL). The organic phases were combined, dried with anhydrous sodium sulfate, and finally purified by silica gel column chromatography (eluent: petroleum ether/ethyl acetate) to obtain the target product 2-mercaptobenzothiazole-6-carbonitrile.

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Yield:315228-79-6 98%

Reaction Conditions:

with iron(III) trifluoride;2,2'-bis-(diphenylphosphino)-1,1'-binaphthyl in N,N-dimethyl-formamide at 110; for 10 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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