反应详情

温度

0 °C

A solution of 5.58 g (9.33 mmol, purity 44%) of the compound from Example 56A in dichloromethane (80 ml) was admixed with 2.60 ml (1.89 g, 18.7 mmol) of triethylamine and then cooled to 0° C. At this temperature, 0.33 ml (0.37 g, 4.67 mmol) of acetyl chloride was added dropwise and the mixture was stirred for 2 h. A further 0.13 ml (0.15 g, 1.86 mmol) of acetyl chloride was added and the mixture was stirred for 1 h. Subsequently, the reaction solution was washed with aqueous 1 N hydrochloric acid, and the organic phase was dried over magnesium sulphate, filtered and concentrated under reduced pressure. The residue was purified by means of column chromatography (silica gel, dichloromethane/methanol 30:1), and the crude product obtained was purified once more by means of preparative HPLC. Yield: 1.17 g (41% of theory)

1. stirringthe mixture was stirred for 1 h
2. washSubsequently, the reaction solution was washed with aqueous 1 N hydrochloric acid
3. dry with materialthe organic phase was dried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by means of column chromatography (silica gel, dichloromethane/methanol 30:1)