反应详情

step 2—To a solution of 322 (88 mg, 0.171 mmol) and HOAc (3 mL) in a 2-5 mL microwave tube was added 48% HBr (0.037 mL, 0.684 mmol). The tube was sealed and heated to 60° for 4 h then to 40° overnight. The reaction was still incomplete so heating at was continued for 6 h at 70°. The reaction was cooled to RT, concentrated and stirred with dilute aq. K2CO3, then twice extracted with EtOAc, dried (MgSO4), filtered and concentrated. The crude product was purified on a SiO2 TLC plate developed with 75% EtOAc/hexane to afford 25 mg (965%) of I-252 as a white solid: MS (M+H)=411.

1. customThe tube was sealed
2. temperatureheated to 60° for 4 h
3. customto 40°
4. customovernight
5. temperatureso heating
6. concentrationconcentrated
7. extractiontwice extracted with EtOAc
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated
11. customThe crude product was purified on a SiO2 TLC plate
12. customto afford 25 mg (965%) of I-252 as a white solid