反应详情

4 M HCl in 1,4-dioxane (6 mL, 24 mmol) was added to tert-butyl 4-(2-(4-methoxyphenoxy)acetyl)-3-((pyridin-3-yloxy)methyl)piperazine-1-carboxylate TFA salt (182 mg, ≦0.305 mmol). After 12 h, the reaction mixture was concentrated under reduced pressure and purified by HPLC (5 to 50% MeCN/0.1% TFA in H2O/0.1% TFA gradient). The desired chomatography fractions were brought to pH ˜12 with 1 N NaOH and were extracted with EtOAc (3×10 mL). The combined organics were dried over Na2SO4, filtered, and concentrated under reduced pressure, yielding 20.9 mg (19%) of the desired product as a thick oil. LC-MS: RT=3.76 min, [M+H]+=358.1.

1. concentrationthe reaction mixture was concentrated under reduced pressure
2. custompurified by HPLC (5 to 50% MeCN/0.1% TFA in H2O/0.1% TFA gradient)
3. extractionwere extracted with EtOAc (3×10 mL)
4. dry with materialThe combined organics were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure