반응 #69896

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4-bromonicotinic acid

MeOH

EDC

→

4-bromonicotinic acid methyl ester

수율 45.6%

용매

DCM

반응 조건

후처리

1. 1
   workup.STIRRINGThe resulting solution was stirred for 3 hours at 0° C
2. 2
   기타The reaction was then quenched with water (100 mL)
3. 3
   추출The resulting solution was extracted with DCM
4. 4
   세척The organic layer was washed with saturated aqueous NaCl (3×100 mL)
5. 5
   건조dried over anhydrous Na2SO4
6. 6
   농축concentrated under vacuum

실험 절차

To a solution of 4-bromonicotinic acid (16.8 g, 83.2 mmol, 1.0 eq.) in DCM (250 mL) at 0° C. was added DMAP (1.0 g, 8.2 mmol, 0.1 eq.). MeOH (2.7 g, 83.7 mmol, 1.0 eq.) was added dropwise with stirring at 0° C. EDC (16.8 g, 87.6 mmol, 1.1 eq.) was then added. The resulting solution was stirred for 3 hours at 0° C. The reaction was then quenched with water (100 mL). The resulting solution was extracted with DCM. The organic layer was washed with saturated aqueous NaCl (3×100 mL), dried over anhydrous Na2SO4 and concentrated under vacuum to yield 4-bromonicotinic acid methyl ester (8.2 g) as a yellow oil.

출처