反应详情

To a suspension of 3.24 g, α-(cyano)-6-fluoro-3,4-dimethoxybenzyl alcohol obtained in Reference Example 1' in 20 ml tetrahydrofuran, was added dropwise 33 ml of 1M solution of borane in tetrahydrofuran with stirring in a methanol/ice bath under an argon gas atmosphere, and the resulting solution was heated under reflux for 3 hours. After cooling the reaction mixture in an ice bath, methanol was added until gas evolution was no longer observed, the resulting solution was stirred at room temperature for 1 hour, and hydrogen chloride gas was introduced until the pH fell below 1. The crystals which separated out were collected, affording 3.34 g of α-(aminomethyl)-6-fluoro-3,4-dimethoxybenzyl alcohol hydrochloride (m.p. 223°-226° C.).

1. temperaturethe resulting solution was heated
2. temperatureunder reflux for 3 hours
3. temperatureAfter cooling the reaction mixture in an ice bath
4. stirringthe resulting solution was stirred at room temperature for 1 hour
5. customThe crystals which separated out
6. customwere collected