تفاعل #9215

معادلة التفاعل

1-(6-bromo-7-hydroxy-2-benzothiazolyl)-3-ethyl-urea

Br2

Toluene

→

1-(4,6-Dibromo-7-hydroxy-2-benzothiazolyl)-3-ethyl-urea

المذيبات

AcOH

ظروف التفاعل

المعالجة

1. 1
   أخرىthe solvents evaporated
2. 2
   أخرىThe crude material was purified by preparative LC/MS
3. 3
   أخرىto give 19 mg (30%) pure 18
4. 4
   أخرىHPLC retention timer 2.90 minutes

الإجراء التجريبي

To a suspension of 1-(6-bromo-7-hydroxy-2-benzothiazolyl)-3-ethyl-urea (50 mg, 0.158 mmol) in AcOH (2 mL) at about 20° C. was added Br2 (9 μl, 0.174 mmol). The reaction mixture was stirred at about 20° C. for about 15 minutes. Toluene (10 mL) was added and the solvents evaporated. The crude material was purified by preparative LC/MS to give 19 mg (30%) pure 18. 1H NMR (DMSO) δ 1.09 (t, 3H, J=6 Hz CH3), 3.19 (m, 2H, CH2), 6.55 (br s, 1H, NH), 7.68 (s, 1H, ArH), 10.51 (br s, 1H, NH or OH), 11.20 (br s, 1H, NH or OH). HPLC retention timer 2.90 minutes.

المصدر