반응 #82963

반응 방정식

methanol

α-(cyano)-6-fluoro-3,4-dimethoxybenzyl alcohol

borane

hydrogen chloride

→

α-(aminomethyl)-6-fluoro-3,4-dimethoxybenzyl alcohol hydrochloride

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   온도the resulting solution was heated
2. 2
   온도under reflux for three hours
3. 3
   온도After cooling the reaction mixture in an ice bath
4. 4
   workup.STIRRINGthe resulting solution was stirred at room temperature for one hour
5. 5
   기타The crystals which separated out
6. 6
   기타were collected

실험 절차

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 three 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 one 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.

출처