反应详情

温度

0 °C

To a dichloromethane (0.03 M) solution of methyl 3-(2-hydroxyethyl)-1-naphthalenecarboxylate (1 eq.) from Step 2, Amine 31 and Hunig's base (1.5 eq.) was added at 0 methanesulfonyl chloride (1.3 eq.). The resulting solution was stirred at 0° C. for 30 min and then at RT for 15 min. The reaction mixture was subsequently quenched with 10% aq. HCl. The aqueous wash was separated and back-extracted with ether. The combined organic extracts were washed further with water and brine, dried over Na2SO4, and filtered. Concentration of the filtrate in vacuo afforded the crude title compound as a colorless oil.

1. waitat RT for 15 min
2. customThe reaction mixture was subsequently quenched with 10% aq. HCl
3. washThe aqueous wash
4. customwas separated
5. extractionback-extracted with ether
6. washThe combined organic extracts were washed further with water and brine
7. dry with materialdried over Na2SO4
8. filtrationfiltered