反应详情

A mixture of 1,1-dimethylethyl N-((4-hydroxy-7-methoxy-2-oxo-2′,3′,5′,6′-tetrahydro-spiro[naphthalene-1,4′-pyran]-3-yl)carbonyl)glycinate (0.36 g, 0.9 mmol) in 2 mL TFA was stirred at room temperature for 30 minutes, M+1=362, M−1=360. The mixture was concentrated and then triturated in DCM/hexane (5:10). The solid was filtered, washed with 10 mL DCM/hexane (5:10), and dried under high vacuum to give 0.3 g of the product as an off-white solid. MS (m/z)=362 (M+H)+. Calculated for C18H19NO7 361.12.

1. concentrationThe mixture was concentrated
2. customtriturated in DCM/hexane (5:10)
3. filtrationThe solid was filtered
4. washwashed with 10 mL DCM/hexane (5:10)
5. customdried under high vacuum