反应详情

To a solution of 302 (0.160 g, 0.270 mmol) and DCM (5 mL) at RT was added 6M HCl in IPA (0.450 mL, 2.70 mmol) and the reaction was stirred for 1 h. The reaction was poured into satd. aq. Na2CO3, and extracted with DCM. The combined organic extracts were dried (MgSO4), filtered, and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with a DCM/MeOH gradient (500:20 to 500:30) to afford 0.010 g (7.74%) of I-76: MS m/z (APCI-pos) M+1=478.

1. additionThe reaction was poured into satd
2. extractionaq. Na2CO3, and extracted with DCM
3. dry with materialThe combined organic extracts were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by SiO2 chromatography
7. washeluting with a DCM/MeOH gradient (500:20 to 500:30)
8. customto afford 0.010 g (7.74%) of I-76