反应详情

温度

50 °C

Methyl 2-propargyloxy-4-(N-t-butyloxycarbonyl-4-piperidinyloxy)benzoate (467 mg, 1.2 mmol) from Step 1 above was dissolved in methanol (10 mL) and to the stirred solution was added 1N NaOH (2.4 mL). The reaction was stirred for 4 h at 50° C. The cooled reaction was acidified with 5% aqueous citric acid (25 mL). The methanol was removed under reduced pressure and the remaining aqueous was extracted with methylene chloride (4×50 mL). The combined organic extracts were washed with water and brine, dried over magnesium sulfate and filtered. The solvent was removed under reduced pressure to give 2-propargyloxy-4-(N-t-butyloxycarbonyl-4-piperidinyloxy)benzoic acid.

1. customThe cooled reaction
2. customThe methanol was removed under reduced pressure
3. extractionthe remaining aqueous was extracted with methylene chloride (4×50 mL)
4. washThe combined organic extracts were washed with water and brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customThe solvent was removed under reduced pressure