反应详情

A solution of 2-1a (0.21 g, 0.51 mmol) and triphenylphosphine (0.133 g, 0.51 mmol) in THF (10mL) was allowed to stir at rt overnight. The reaction was quenched with water (10 mL) and heated at 60° C. for 1 h. The product was extracted with EtOAc (2×30 mL) and washed with brine (30 mL), dried over MgSO4, filtered and concentrated. The remaining oil was dissolved in CH2CL2 (5 mL)I TFA (2 mL) and allowed to stir at rt overnight. The solvent was removed in vacuo. The remaining oil was dissolved in CH3CN (3 mL) and purified on a Gilson automated system affixed with a YMC J'sphere H80 30×100 mm column (eluting with 5-95% CH3CN +0.1% TFA in water +0.1% TFA over 20 min) to afford pure 2-3a.

1. customThe reaction was quenched with water (10 mL)
2. temperatureheated at 60° C. for 1 h
3. extractionThe product was extracted with EtOAc (2×30 mL)
4. washwashed with brine (30 mL)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. dissolutionThe remaining oil was dissolved in CH2CL2 (5 mL)I TFA (2 mL)
9. stirringto stir at rt overnight
10. customThe solvent was removed in vacuo
11. dissolutionThe remaining oil was dissolved in CH3CN (3 mL)
12. custompurified on a Gilson automated system
13. washaffixed with a YMC J'sphere H80 30×100 mm column (eluting with 5-95% CH3CN +0.1% TFA in water +0.1% TFA over 20 min)
14. customto afford pure 2-3a