反应详情

温度

115 °C

The product from Example 77A was mixed with the product from Example 59C (135 mg, 0.35 mmol) in 2-methoxyethanol (1.2 mL) and N,N-diisopropylethylamine (0.74 mL, 1.74 mmol), then heated at 115° C. overnight, then cooled, diluted with CH2Cl2, and washed with 1 M NaOH. The aqueous layer was extracted with CH2Cl2. The combined organic extracts were dried (MgSO4), filtered, concentrated and purified by chromatography on silica gel, eluting with a gradient of 1:0 to 1:2 CH2Cl2:[10% (9:1 MeOH:saturated aqueous ammonium hydroxide)] to provide the title compound. MS (M+H)+ m/z 426.

1. temperaturecooled
2. washwashed with 1 M NaOH
3. extractionThe aqueous layer was extracted with CH2Cl2
4. dry with materialThe combined organic extracts were dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified by chromatography on silica gel
8. washeluting with a gradient of 1:0 to 1:2 CH2Cl2