147118-36-3

Hazard Information

Questions And Answer

• Synthesis

  To a 500 mL three-necked flask, add 270 mL of tetrahydrofuran, 9.0 g (240 mmol) of sodium borohydride, and 22.8 g (60 mmol) (HPLC: 99.7%) of pyrimidinyl ester (II). Cool to 0 °C, and slowly add 34.2 g (240 mmol) of boron trifluoride diethyl ether complex. Heat to 60 °C and maintain the reaction temperature for 20 h. After the reaction is complete, cool to room temperature, and slowly add hydrochloric acid (v/v = 5%) to the reaction mixture. Stir for 1.5 h, then add saturated NaHCO3 to adjust the pH to 7–8. Extract with CH2Cl2 (60 mL × 2), separate the aqueous layer, dry the CH2Cl2 layer with anhydrous sodium sulfate, filter, and concentrate the filtrate to dryness under reduced pressure to obtain a pale yellow solid pyrimidinol (III). The yield was 20.49 g of 4-(4-Fluorophenyl)-6-isopropyl-2-[(N-methyl-n-methylsulfonyl)amino]pyrimidine-5-yl-methanol, with a yield of 96.7%.;

Spectrum Detail

Supplier

Related Products