反应详情

温度

120 °C

A mixture of 20 g (0.110 mol) of 73 and 100 ml of conc. sulphuric acid was heated to 120° C. for 4 h. After cooling the mixture was poured over ice followed by basification with ammonia. Extraction with 3×400 ml of dichloromethane, drying of the combined organic phase over magnesium sulphate, and removal of the solvent in vacuo gave crude 74 as a red oil, which was sufficiently pure. Yield: 17 g (0.100 mol, 97%).

1. temperatureAfter cooling the mixture
2. additionwas poured over ice
3. extractionExtraction with 3×400 ml of dichloromethane
4. dry with materialdrying of the combined organic phase over magnesium sulphate, and removal of the solvent in vacuo