反应详情

温度

5 °C

Into a 250-mL 3-necked round-bottom flask was placed a solution of 113j (18 g, 74.01 mmol, 1.00 equiv) in ethanol (100 mL), followed by the addition of NaBH4 (2.8 g, 74.02 mmol, 1.00 equiv) in several batches at 0° C. (FIG. 14). The resulting solution was stirred at 5° C. for 10 min, quenched by the addition of 50 mL of saturated aqueous NH4Cl, concentrated under vacuum and extracted with 3×50 mL of ethyl acetate. The combined organic layers were washed with 1×100 mL of water and 1×100 mL of brine, dried over anhydrous sodium sulfate and concentrated under vacuum to afford 18 g (99%) of 113k as a white solid.

1. customInto a 250-mL 3-necked round-bottom flask was placed
2. customquenched by the addition of 50 mL of saturated aqueous NH4Cl
3. concentrationconcentrated under vacuum
4. extractionextracted with 3×50 mL of ethyl acetate
5. washThe combined organic layers were washed with 1×100 mL of water and 1×100 mL of brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated under vacuum