反应详情

The product of step (b) (˜165 mmol, ˜42 g) was dissolved in 1 L of DCM. DMF (100 uL) was added followed slowly by oxalyl chloride (21.7 mL, 247 mmol). After 1 hour, the reaction was concentrated to dryness and the crude material was re-dissolved in DCE (1 L). AlCl3 (55 g, 410 mmol) was carefully added and the reaction was stirred at room temperature for ½ hour. The crude reaction was quenched with ice, washed with water (3×), and dried over MgSO4. The title product was purified by silica gel chromatography (30% EtOAc in Hexanes) to give 10.5 grams of the sub-title compound as a white solid. MS: ESI (positive): 240 (M+H).

1. concentrationthe reaction was concentrated to dryness
2. dissolutionthe crude material was re-dissolved in DCE (1 L)
3. customThe crude reaction
4. customwas quenched with ice
5. washwashed with water (3×)
6. dry with materialdried over MgSO4
7. customThe title product was purified by silica gel chromatography (30% EtOAc in Hexanes)