反应详情

温度

0 °C

1.00 g (4.47 mmol) of the compound from example 34A is initially charged in 15 ml of chloroform, and 1.5 ml (16.10 mmol) of phosphoryl chloride are added carefully. With stirring, the reaction mixture is heated at reflux for 30 min. The mixture is then cooled to 0° C. and made weakly basic by addition of aqueous ammonia. The mixture is extracted three times with in each case 20 ml of ethyl acetate. The combined organic phases are washed twice with in each case 5 ml of water and then dried over magnesium sulphate. The solvent is removed on a rotary evaporator. Without further purification, the product obtained in this manner is used for the subsequent reactions.

1. temperaturethe reaction mixture is heated
2. temperatureat reflux for 30 min
3. extractionThe mixture is extracted three times with in each case 20 ml of ethyl acetate
4. washThe combined organic phases are washed twice with in each case 5 ml of water
5. dry with materialdried over magnesium sulphate
6. customThe solvent is removed on a rotary evaporator
7. customWithout further purification
8. customthe product obtained in this manner