反応 #595371

反応方程式

H2SO4

CO2

n-BuLi

diisopropylamine

1,4-difluoro-2-methoxybenzene

LDA

→

title compound

3,6-difluoro-2-methoxybenzoic acid

溶媒

diethyl ether

THF

THF

反応条件

後処理

1. 1
   その他the resulting precipitate was collected
2. 2
   洗浄washed with H2O
3. 3
   その他dried

実験手順

A solution of 1,4-difluoro-2-methoxybenzene (i-6a) (2.88 g, 20 mmol) in THF (5 mL) was added to a solution of LDA freshly prepared from n-BuLi (10M solution in hexane, 2.2 mL, 22 mmol) and diisopropylamine (2.28 g, 22.8 mmol) in THF (20 mL) at −60° C. After 30 min, a freshly prepared solution of CO2 in diethyl ether (20 mL) was quickly added. Then aq. H2SO4 was added, and the resulting precipitate was collected and washed with H2O, and dried to give the title compound (i-6b) as white crystals. LCMS (ESI) calc'd for C8H6F2O3 [M+H]+: 189. found: 189.

出典