HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethyl orthoformate → HCID 19855426, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethyl orthoformate | HCID 9005 | — |
| Reactant | (3R,4R)-3-(2,4-Dihydroxyphenyl)-4-(3-hydroxypropyl)cyclohexan-1-one | HCID 70360050 | — |
| Catalyst | Sulfuric Acid | HCID 1118 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 19855426 | HCID 19855426 | 82% |
Reaction Steps
A solution of 1.5 g. (5.68 mmole) of trans-3-(2,4-dihydroxyphenyl)-4-(3-hydroxypropyl)cyclohexanone in 40 ml. methanol, 6 ml. trimethylorthoformate and 7 drops of concentrated sulfuric acid was stirred at 0° C. for 45 minutes. The reaction was quenched by the addition of excess solid sodium bicarbonate and then evaporated on a rotovapor. The residue was diluted with 300 ml. saturated sodium bicarbonate-300 ml. ether. The ether extract was dried over magnesium sulfate and evaporated. The crude product was purified via column chromatography on 150 g. of silica gel eluted in 15 ml. fractions with ether to yield 1.29 g. (82%) of the title compound as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04831059 |
| Source dataset | uspto-grants-1989_05 |
| ORD ID | ord-91c38c0c7796473fa640a12f919f0ce1 |
| Source note | uspto-grants-1989_05 |