反应详情

To a 100 mL round bottom flask was charged with acid 101a (630 mg, 3.3 mmol) in CH2Cl2 (20 mL) was added oxalyl chloride (4.9 mL, 9.8 mmol, 2.0M solution in CH2Cl2) followed by DMF (1 drop). After the reaction was stirred at room temperature for 8 h, it was concentrated. To the residue was added Et2O (25 mL) and the mixture was concentrated. This repeated to removed any excess oxalyl chloride. The residue was dissolved in CH2Cl2 (15 mL) and EtOH (15 mL). After the reaction was stirred at room temperature for 30 min, it was concentrated. The residue was dissolved in EtOAc (15 mL) and this organic phase was washed with aqueous HCl (15 mL, 1M), H2O (15 mL), brine (15 mL), dried with Na2SO4 and concentrated. The crude 101b (660 mg, 91%) was used without further purification.

1. concentrationit was concentrated
2. additionTo the residue was added Et2O (25 mL)
3. concentrationthe mixture was concentrated
4. customto removed any excess oxalyl chloride
5. dissolutionThe residue was dissolved in CH2Cl2 (15 mL)
6. stirringAfter the reaction was stirred at room temperature for 30 min
7. concentrationit was concentrated
8. dissolutionThe residue was dissolved in EtOAc (15 mL)
9. washthis organic phase was washed with aqueous HCl (15 mL, 1M), H2O (15 mL), brine (15 mL)
10. dry with materialdried with Na2SO4
11. concentrationconcentrated
12. customThe crude 101b (660 mg, 91%) was used without further purification