تفاعل #9207

معادلة التفاعل

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

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

potassium carbonate

methanol

→

desired product

1-(7-Hydroxy-2-benzothiazolyl)-3-ethyl-urea

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas cooled down to about 0° C
2. 2
   workup.STIRRINGwas stirred at about 0–85° C. for about 16 hours
3. 3
   ترشيحThe solid was filtered off
4. 4
   غسيلwashed with methanol
5. 5
   أخرىThe solvent was evaporated
6. 6
   workup.DISSOLUTIONthe residue was dissolved in DMF
7. 7
   أخرىThe crude reaction solution
8. 8
   أخرىwas purified by preparature LC/MS

الإجراء التجريبي

General Procedure for 1-(6-bromo-7-alkoxy-2-benzothiazolyl)-3-ethyl-urea compounds 9–13. A mixture of 1-(6-bromo-7-hydroxy-2-benzothiazolyl)-3-ethyl-urea 6 and potassium carbonate (1.05 eq) in anhydrous DMF was stirred at about 20° C. for about 0.5 hour, and was cooled down to about 0° C. The mixture was treated with an alkyl halide (1.0 eq), and was stirred at about 0–85° C. for about 16 hours. To the reaction mixture was added methanol. The solid was filtered off and washed with methanol. The solvent was evaporated and the residue was dissolved in DMF. The crude reaction solution was purified by preparature LC/MS to give pure desired product.

المصدر