반응 #46177

반응 방정식

5-bromo-2,2-difluoro-benzo[1,3]dioxole

acetonitrile

triethylamine

→

2,2-difluoro-benzo[1,3]dioxole-5-carboxylic acid methyl ester

용매

methanol

반응 조건

후처리

1. 1
   기타The cooled reaction mixture
2. 2
   여과was filtered
3. 3
   기타the filtrate was evaporated to dryness
4. 4
   기타The residue was purified by silica gel column chromatography

실험 절차

A solution of 5-bromo-2,2-difluoro-benzo[1,3]dioxole (11.8 g, 50.0 mmol) and tetrakis(triphenylphosphine)palladium (0) [Pd(PPh3)4, 5.78 g, 5.00 mmol] in methanol (20 mL) containing acetonitrile (30 mL) and triethylamine (10 mL) was stirred under a carbon monoxide atmosphere (55 PSI) at 75° C. (oil bath temperature) for 15 hours. The cooled reaction mixture was filtered and the filtrate was evaporated to dryness. The residue was purified by silica gel column chromatography to give crude 2,2-difluoro-benzo[1,3]dioxole-5-carboxylic acid methyl ester (11.5 g), which was used directly in the next step.

출처