تفاعل #1184100

معادلة التفاعل

chloroform

5-Bromo-nicotinic acid

CHCl3

WSC HCl

→

5-Bromo-nicotinic acid tert-butyl ester

المذيبات

tert-BuOH

ظروف التفاعل

المعالجة

1. 1
   غسيلwashed with 0.5N HCl aq. (220 mL), 0.5N NaOH aq. (100 mL), brine
2. 2
   تجفيفdried over MgSO4 and silica gel
3. 3
   ترشيحAfter filtration
4. 4
   أخرىthe solvents were removed in vacuo

الإجراء التجريبي

5-Bromo-nicotinic acid (20.2 g, 100 mmol) was dissolved in CHCl3 (200 mL) and tert-BuOH (40 mL); and WSC-HCl (21.1 g, 110 mmol) and DMAP (21.1 g, 110 mmol) was added thereto in order, and stirred at room temperature over night. The reaction mixture was diluted with chloroform, washed with 0.5N HCl aq. (220 mL), 0.5N NaOH aq. (100 mL), brine and dried over MgSO4 and silica gel. After filtration, the solvents were removed in vacuo to afford 5-Bromo-nicotinic acid tert-butyl ester as a colorless solid. This solid was used for the next step without further purification.

المصدر