反应详情

温度

0 °C

To a suspension of NaH (60% in mineral oil, 8.4 g, 0.21 mol) in THF (200 mL) was added dropwise a solution of 2-tert-butyl-4-methylphenol (33 g, 0.20 mol) in THF (100 mL) at 0° C. The mixture was stirred at 0° C. for 15 min and then phosphorochloridic acid diethyl ester (37 g, 0.2.1 mol) was added dropwise at 0° C. After addition, the mixture was stirred at ambient temperature for 30 min. The reaction was quenched with sat. NH4Cl (300 mL) and then extracted with Et2O (350 mL×2). The combined organic layers were washed with brine, dried over anhydrous Na2SO4, and then evaporated under vacuum to give 2-tert-butyl-4-methylphenyl diethyl phosphate (contaminated with mineral oil) as a colorless oil (60 g, 100%), which was used directly in the next step.

1. additionAfter addition
2. stirringthe mixture was stirred at ambient temperature for 30 min
3. customThe reaction was quenched with sat. NH4Cl (300 mL)
4. extractionextracted with Et2O (350 mL×2)
5. washThe combined organic layers were washed with brine
6. dry with materialdried over anhydrous Na2SO4
7. customevaporated under vacuum