반응 #442934
ord-78d674f32e24418bba7339b86ba6f044
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타After evaporation of the solvent
- 2기타the residual oil was purified by preparative thin layer chromatography (1 mm thick plate, CH2Cl2 /MeOH: 10/1)
실험 절차
A mixture of 17-cyclopropylmethyl-3,14β-dihydroxy-4,5α-epoxy-6α-(N-methoxy-3,4-dichlorophenylacetamido)morphinan (197 mg, 0.35 mmol), trimethylsilyldiazomethane (10% solution in CH2Cl2, 0.57 g, 0.5 mmol), diisopropylethylamine (65 mg, 0.5 mmol), methanol (0.2 ml), and acetonitrile (2 ml) was stirred at room temperature for 13 h. After evaporation of the solvent, the residual oil was purified by preparative thin layer chromatography (1 mm thick plate, CH2Cl2 /MeOH: 10/1) to give 47 mg of amorphous solid. This was purified again by preparative thin layer chromatography (1 mm thick plate, CH2Cl2 /MeOH: 10/1) to give 25 mg of amorphous solid as desired product.