反应详情

温度

80 °C

A mixture of 428A (44 mg, 0.10 mmol), Et3N (28 μl, 0.20 mmol) and DPPA (43 μl, 0.20 mmol) in dioxane (1.5 ml) was stirred under argon overnight. TMSN3 (27 μl, 0.20 mmol) was added and the mixture was heated to 80° C. for 2 h, then cooled to rt. 2-Morpholin-4-yl-ethylamine (26 μl, 0.20 mmol) was added and the mixture was heated to 80° C. for 2 h, then cooled to rt. Removal of the solvent followed by flash chromatography of the residue on silica gel (3%-5% MeOH—CH2Cl2) gave a gray solid. Recrystalization of the solid in CH2Cl2/pentane gave 428 (43 mg, 75%) as a light yellow solid. It has a retention time of 3.93 min (standard LC1 method, 8 min run). MS Found: (M+H)+=566.1

1. temperaturecooled to rt
2. temperaturethe mixture was heated to 80° C. for 2 h
3. temperaturecooled to rt
4. customRemoval of the solvent
5. customgave a gray solid
6. customRecrystalization of the solid in CH2Cl2/pentane