تفاعل #556496

معادلة التفاعل

2-amino-4-methylbenzothiazole

sodium nitrite

→

4-methyl-3H-benzothiazol-2-one

المذيبات

formic acid

acetic acid

hydrochloric acid

water

water

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGThe reaction mixture was stirred for 20 min at this temperature
2. 2
   درجة الحرارةrefluxed overnight
3. 3
   استخلاصextracted several times with EtOAc
4. 4
   غسيلThe combined organic phases were washed with saturated sodium chloride solution
5. 5
   أخرىdried on sodium sulphate
6. 6
   ترشيحfiltered
7. 7
   أخرىthe filtrate was evaporated down

الإجراء التجريبي

5.00 g (30.5 mmol) 2-amino-4-methylbenzothiazole in 15.0 mL formic acid, 6.10 mL glacial acetic acid and 112 mL conc. hydrochloric acid were cooled to −5° C. with stirring and slowly combined with a solution of 2.10 g (30.5 mmol) sodium nitrite in 5.0 mL water. The reaction mixture was stirred for 20 min at this temperature, then heated to RT and then refluxed overnight. The cooled mixture was then mixed with water and extracted several times with EtOAc. The combined organic phases were washed with saturated sodium chloride solution, dried on sodium sulphate, filtered and the filtrate was evaporated down.

المصدر