Reacción #2029113

Ecuación de reacción

ammonia

(3,5-diiodo-phenyl)-thiourea

Br2

→

desired product

Rendimiento 88.0%

5,7-Diiodo-benzothiazol-2-ylamine

Rendimiento 88.0%

Disolventes

H2O

CHCl3

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturaby refluxing at 70-75° C. for 3 h
2. 2
   TemperaturaThe reaction mixture was cooled to room temperature
3. 3
   Filtraciónfiltered
4. 4
   Otroto get the crude residue that
5. 5
   Lavadowas washed with hexane and diethyl ether
6. 6
   OtroThe solid thus obtained
7. 7
   workup.STIRRINGstirred for 30 min
8. 8
   OtroThe solid thus obtained
9. 9
   Filtraciónwas filtered
10. 10
    Lavadowashed with water

Procedimiento

To a solution of (3,5-diiodo-phenyl)-thiourea (4.0 g, 0.01 mol) in CHCl3 (160 mL) at −55-60° C. was added dropwise a solution of Br2 (4.72 g, 0.02 mol, in 25 ml of CHCl3) over a period of 15 min. The reaction mixture was stirred at −55-60° C. for 15 min followed by refluxing at 70-75° C. for 3 h. The reaction mixture was cooled to room temperature and filtered to get the crude residue that was washed with hexane and diethyl ether. The solid thus obtained was dissolved in H2O, basified with aqueous ammonia solution to pH 10-12 and stirred for 30 min. The solid thus obtained was filtered and washed with water to get the desired product (3.50 g, 88%).

Fuente