反应详情

温度

5 °C

2-Ethylsulfonyl-5-trifluoromethylpyrimidine (4.7 mmol) was added to 1M NaOH, the mixture stirred at 5° C. for 10 min, then at room temperature for 10 min and finally the pH was adjusted to 2 with HCl. After filtration the filtrate was evaporated, the residue dried and extracted with benzene, the benzene solution evaporated, the residue extracted with boiling ethyl acetate, (3×40 ml), and the ethyl acetate solution evaporated to yield the product; yield 0.50 g (67%). For final purification the product was sublimed at 110°-120° C./0,01 mmHg; m.p. 154° C., 1H NMR (DMSO-d6): δ 8.50 (H-4, H-6), MS [70 eV; m/z (% rel. int.)] 164 (99, M), 145 (21), 136 (100), 117 (25), 116 (16), 109 (11), 90 (28), 89 (40), 75 (35). IR (KBr): 1690 cm-1 (CO).

1. waitat room temperature for 10 min
2. filtrationAfter filtration the filtrate
3. customwas evaporated
4. customthe residue dried
5. extractionextracted with benzene
6. customthe benzene solution evaporated
7. extractionthe residue extracted with boiling ethyl acetate, (3×40 ml),
8. customthe ethyl acetate solution evaporated
9. customto yield the product
10. customFor final purification the product
11. customwas sublimed at 110°-120° C.