* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Reference：
[1] Helvetica Chimica Acta, 1942, vol. 25, p. 515,519
2
[ 5464-79-9 ]
[ 3507-27-5 ]
Yield
Reaction Conditions
Operation in experiment
69%
With copper dichloride; isopentyl nitrite In acetonitrile at 65℃; for 2 h; Inert atmosphere
A 500 mL three-necked flask equipped with a condenser under nitrogen was charged with copper(II) chloride (3.36 g, 25.0 mmol), MeCN (71 mL) and isopentyl nitrite (2.2 mL, 16.6 mmol). The suspension was stirred in a 65 °C oil bath for 10 mm before adding a solution of 2- amino-4-methoxybenzothiazole (2.00 g, 11.1 mmol) in MeCN (42 mL). The reaction mixture was stirred in a 65 °C oil bath for 2 h and it was allowed to cool down at 20 °C. Water (150 mL) and iN HC1 (100 mL) were added and the resulting mixture was extracted with EtOAc (3 x 100 mL). Combined organic layers were washed with brine, dried over anhydrous Na2SO4, filtered and concentrated. The obtained residue was purified by Si02 chromatography (EtOAc in hexanes, 5 to 15percent gradient) to afford the title compound (1.52 g, 69percent) as a white solid.
With copper dichloride; isopentyl nitrite; In acetonitrile; at 65℃; for 2h;Inert atmosphere;
A 500 mL three-necked flask equipped with a condenser under nitrogen was charged with copper(II) chloride (3.36 g, 25.0 mmol), MeCN (71 mL) and isopentyl nitrite (2.2 mL, 16.6 mmol). The suspension was stirred in a 65 C oil bath for 10 mm before adding a solution of 2- amino-4-methoxybenzothiazole (2.00 g, 11.1 mmol) in MeCN (42 mL). The reaction mixture was stirred in a 65 C oil bath for 2 h and it was allowed to cool down at 20 C. Water (150 mL) and iN HC1 (100 mL) were added and the resulting mixture was extracted with EtOAc (3 x 100 mL). Combined organic layers were washed with brine, dried over anhydrous Na2SO4, filtered and concentrated. The obtained residue was purified by Si02 chromatography (EtOAc in hexanes, 5 to 15% gradient) to afford the title compound (1.52 g, 69%) as a white solid.
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