反应详情

温度

100 °C

2.52 g (10 mmol) of 4-chloro-2,6-di-pyrrolidin-1-yl-pyrimidine (J. Med. Chem. (1990) 33 (4), 1145-1151) and 2.07 g (10 mmol) of 4-nitrophenylpiperazine are dissolved in a 250 ml flask containing 20 ml of anhydrous pyridine, under an argon atmosphere. The reaction mixture is heated at 100° C. for 48 hours. After cooling down, the contents of the flask are poured into 250 ml of water and the product is extracted using twice 50 ml of CH2Cl2. The organic phase is then washed with 50 ml of brine, dried over magnesium sulphate, filtered and concentrated under vacuum. The residue is purified on a silica column (eluent: Heptane/AcOEt: 2/1). An orange solid is obtained with a yield of 49%. Melting point: 200-201° C.

1. temperatureAfter cooling down
2. extractionthe product is extracted
3. washThe organic phase is then washed with 50 ml of brine
4. dry with materialdried over magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe residue is purified on a silica column (eluent: Heptane/AcOEt: 2/1)
8. customAn orange solid is obtained with a yield of 49%