反应详情

Crude methyl 3-fluoro-4-(oxetan-3-yloxy)benzoate from Step 1, MeOH (1 mL), and KOH (4.0 mL of 3.0 M, 12 mmol) were combined and the mixture was allowed to stir for 3 h at rt. The mixture was extracted with EtOAc and the organic layer was discarded. The aqueous layer was then treated with 1N HCl and the pH was adjusted to pH 3. The aqueous layer was extracted with EtOAc (3×) and the combined organic layers were dried over sodium sulfate and the solvent was removed. The crude acid was used without further purification. ESI-MS m/z calc. 212.1. found 213.0 (M+1)+; Retention time: 1.65 minutes (4 min run).

1. extractionThe mixture was extracted with EtOAc
2. additionThe aqueous layer was then treated with 1N HCl
3. extractionThe aqueous layer was extracted with EtOAc (3×)
4. dry with materialthe combined organic layers were dried over sodium sulfate
5. customthe solvent was removed
6. customThe crude acid was used without further purification
7. customRetention time: 1.65 minutes (4 min run)