HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3'-(Hydroxymethyl)-2,3,5,6-tetramethylbiphenyl-4-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 4'-Hydroxy-2',3',5',6'-tetramethylbiphenyl-3-carbaldehyde | HCID 59342590 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3'-(Hydroxymethyl)-2,3,5,6-tetramethylbiphenyl-4-ol | HCID 59342613 | 93% |
Reaction Steps
A solution of 4′-hydroxy-2′,3′,5′,6′-tetramethylbiphenyl-3-carbaldehyde (2.03 g, 8.00 mmol) in a mixed solvent of methanol (10 mL) and tetrahydrofuran (20 mL) was ice-cooled, sodium borohydride (90%, 0.336 g, 8.00 mmol) was added, and the mixture was stirred for 2 hr under nitrogen atmosphere. The reaction mixture was treated with diluted hydrochloric acid, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained crystals were recrystallized from heptane-ethyl acetate to give the title compound (1.90 g, yield 93%) as colorless crystals. melting point 152-153° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07732626B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-38e8e7a174a34e359819d104e8773c02 |
| Source note | uspto-grants-2010_06 |