HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Methyl 4-(hydroxymethyl)-2-nitrobenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Methyl hydrogen 2-nitroterephthalate | HCID 98592 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Methyl 4-(hydroxymethyl)-2-nitrobenzoate | HCID 22672700 | 63% |
Reaction Steps
Tetrahydrofuran solution of 1.0M borane-tetrahydrofuran complex was added dropwise to tetrahydrofuran solution (45 mL) of 2.25 g of 4-methoxycarbonyl-3-nitrobenzoic acid and stirred at room temperature for 48 hours. Methylalcohol (2 ml) and 1N hydrochloric acid (10 ml) were added thereto and concentrated. After ethyl acetate and water were added, liquid separation was conducted. The organic layer was washed with saturated sodium hydrogen carbonate and dried over sodium sulfate. After removing the solvent, the obtained crude material was purified with silica gel column chromatography to obtain 1.33 g of methyl 4-hydroxymethyl-2-nitrobenzoate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08309561B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-fbe48c56163a46d1ad449a5c9bfb3e35 |
| Source note | uspto-grants-2012_11 |