HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-Fluoro-4-hydroxymethylbenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | Methyl 4-cyano-2-fluorobenzoate | HCID 15278726 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 3-Fluoro-4-hydroxymethylbenzonitrile | HCID 11480543 | — |
Reaction Steps
16.10 g (89.9 mmol) of methyl 4-cyano-2-fluorobenzoate are dissolved in 150 ml of methanol. Then 3.40 g (89.9 mmol) of sodium borohydride are added in portions. After the reaction has taken place (TLC check), the mixture is adjusted to pH 3 with dilute hydrochloric acid and extracted several times with dichloromethane. The combined organic phases are washed with saturated sodium chloride solution and dried with magnesium sulfate. The solvent is then removed in vacuo, and the residue is purified by column chromatography (silica gel, mobile phase: cyclohexane/ethyl acetate 15:1→3:7). 3.70 g (27.2% of theory) of the title compound are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09051316B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-a8e3a28fe74d446d8053dd403963a03f |
| Source note | uspto-grants-2015_06 |