反应详情

To LAH (1 M/Et2O, 104.4 ml, 104.4 mmol) in anhydrous THF (300 ml) at 0° C. was added methyl 5-chloro-2-cyanobenzoate (9.28 g, 0.512 mmol) maintaining the temperature below 20° C. After one half hour, quenched at OC with water (3.97 ml), NaOH (1N, 11.9 ml, 11.9 mmol) and water (3.97 ml). A precipitate was filtered out and washed with THF. The filtrate was concentrated in vacuo and was used immediately in the next step.

1. temperaturemaintaining the temperature below 20° C
2. waitAfter one half hour
3. filtrationA precipitate was filtered out
4. washwashed with THF
5. concentrationThe filtrate was concentrated in vacuo