HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → alpha-(Aminomethyl)-6-fluoro-3,4-dimethoxybenzyl alcohol hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Borane | HCID 6331 | — |
| Reactant | 2-(2-Fluoro-4,5-dimethoxyphenyl)-2-hydroxyacetonitrile | HCID 3833943 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | alpha-(Aminomethyl)-6-fluoro-3,4-dimethoxybenzyl alcohol hydrochloride | HCID 14719567 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05623074 |
| Source dataset | uspto-grants-1997_04 |
| ORD ID | ord-2436083a0b37474581de189c1fe3f65d |
| Source note | uspto-grants-1997_04 |