反应详情

温度

0 °C

Under nitrogen atmosphere 4-methanesulfonyloxy-benzoic acid methyl ester (2.3 g, 10 mmol) was dissolved in dry THF (50 mL) and LiAlH4 (0.28 g, 10 mmol) was added at 0° C. After the addition was completed the ice bath was removed and stirring was continued at r.t. for 2 h. The mixture was cooled down to 0° C. again and excess LiAlH4 was hydrolyzed by the addition of MeOH, H2O and aq. HCl (2N). After extracting DCM the combined organic layers were dried (MgSO4) and evaporated under reduced pressure to afford the crude but mainly pure product as an oil which was used in the next step without further purification (1.95 g, 96.4%). 1H NMR (400 MHz, CDCl3): δ 7.35-7.37 (d, 2H), 7.21-7.23 (d, 2H), 4.65 (s, 2H), 3.09 (s, 3H).

1. additionAfter the addition
2. customwas removed
3. additionexcess LiAlH4 was hydrolyzed by the addition of MeOH, H2O and aq. HCl (2N)
4. extractionAfter extracting DCM the combined organic layers
5. dry with materialwere dried (MgSO4)
6. customevaporated under reduced pressure
7. customto afford the crude but mainly pure product as an oil which
8. customwas used in the next step without further purification (1.95 g, 96.4%)