反应详情

To a solution of Compound 260a (100 mg, 0.40 mmol) in methanol (10 mL) stirred at r.t., was added DMT-MM (4-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride, 142 mg, 0.52 mmol), N-methylmorpholine (88.4 μL, 0.81 mmol) and N,O-dimethylhydroxylamine hydrochloride (60 mg, 0.615 mmol). The reaction mixture was stirred at r.t. for 3 h. The solvent was evaporated to dryness in vacuo. The residue was diluted with aq. 1N NaOH and dichloromethane. The combined organic layers were washed with brine, dried on Na2SO4 and evaporated to dryness in vacuo to afford a residue, which was purified by flash chromatography (EtOAc—Petroleum Ether 60:40) affording the title product (90 mg).

1. customThe solvent was evaporated to dryness in vacuo
2. additionThe residue was diluted with aq. 1N NaOH and dichloromethane
3. washThe combined organic layers were washed with brine
4. customdried on Na2SO4
5. customevaporated to dryness in vacuo
6. customto afford a residue, which
7. customwas purified by flash chromatography (EtOAc—Petroleum Ether 60:40)