反应详情

温度

110 °C

To a solution of 7 (49 mg, 0.1 mmol) in 1,2-dimethoxyethane (DME, 2 mL) and EtOH (1 mL) was added 37 (31 mg, 0.12 mmol), 0.5 M NaHCO3 (1 mL). The suspension was bubbled with argon for 5 min before adding Pd(PPh3) (38, 12 mg, 0.01 mmol). The reaction mixture was heated at 110° C. for 30 min using microwave initiator. The solid was filtered off and the filtrate was extracted with EtOAc (10 ml×2). The combined organic layers were dried (Na2SO4) and concentrated in vacuo. The compound 39 was purified by HPLC. The 39 was dissolved in CH2Cl2 (2 ml) and TFA (0.5 ml) was added. The mixture was stirred for 2 h at r.t. The solvent was removed in vacuo. The residue was treated with MeOH (2 mL) and the solid was collected by centrifuge and washed with MeOH. Compound 40 (20 mg, 48%) was obtained as yellow solid. LC-MS: calcd. for C21H12N2O4S2: 419 (M−1).

1. customThe suspension was bubbled with argon for 5 min
2. filtrationThe solid was filtered off
3. extractionthe filtrate was extracted with EtOAc (10 ml×2)
4. dry with materialThe combined organic layers were dried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customThe compound 39 was purified by HPLC
7. dissolutionThe 39 was dissolved in CH2Cl2 (2 ml)
8. additionTFA (0.5 ml) was added
9. customThe solvent was removed in vacuo
10. additionThe residue was treated with MeOH (2 mL)
11. customthe solid was collected by centrifuge
12. washwashed with MeOH