反应详情

To a solution of the diol heptyne of Step 6 isomer (2.85 mmol) in CH2Cl2 (5.5 mL) was added trifluoroacetic acid (71.3 mmol). The reaction was monitored by TLC (50% EtOAc in hexane). After 30 minutes the solution was concentrated and an aqueous 1.0N NaOH solution (7 mL) was added. The solution was extracted with EtOAc (4×10 mL). The organic layer was dried with MgSO4. The filtrate was concentrated to give the title amine as a white sticky solid (0.67 g, 100% yield). The 1H, 13C and APT NMR spectral data were consistent with the prepared structure.

1. concentrationAfter 30 minutes the solution was concentrated
2. additionan aqueous 1.0N NaOH solution (7 mL) was added
3. extractionThe solution was extracted with EtOAc (4×10 mL)
4. dry with materialThe organic layer was dried with MgSO4
5. concentrationThe filtrate was concentrated