تفاعل #595371
ord-5aafd660425941529d5bb7699d4bd151
معادلة التفاعل
H2SO4
CO2
n-BuLi
diisopropylamine
1,4-difluoro-2-methoxybenzene
LDA
→
title compound
3,6-difluoro-2-methoxybenzoic acid
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىthe resulting precipitate was collected
- 2غسيلwashed with H2O
- 3أخرىdried
الإجراء التجريبي
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.