反应详情

Methyl 3-[(dimethylamino)methyl]-5-fluorobenzoate (0.040 g, 0.19 mmol from Step 3) was dissolved in tetrahydrofuran (3 mL) and lithium hydroxide monohydrate (0.0954 g, 2.27 mmol) dissolved in water (1 mL) was added. The reaction was stirred for 3 hours. The crude reaction mixture was purified by preparative HPLC-MS (C18, eluting with a gradient of H2O/MeCN containing 0.15% NH4OH). The eluent containing the desired mass was evaporated using rotary evaporation to afford product (22 mg, 59%), which was used directly in Step 5. LCMS (M+H)+: 198.1.

1. additionwas added
2. customThe crude reaction mixture
3. customwas purified by preparative HPLC-MS (C18
4. washeluting with a gradient of H2O/MeCN containing 0.15% NH4OH)
5. additionThe eluent containing the desired mass
6. customwas evaporated
7. customevaporation