HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4,5,6,7-Tetrahydro-3-hydroxy-1(3H)-isobenzofuranone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 3,4,5,6-Tetrahydrophthalic anhydride | HCID 12475 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4,5,6,7-Tetrahydro-3-hydroxy-1(3H)-isobenzofuranone | HCID 10909777 | — |
Reaction Steps
To a solution of 1-cyclohexene-1,2-dicarboxylic anhydride (25.2 g) in tetrahydrofuran (125 mL) at 0° C. was added sodium borohydride (1.51 g). The mixture was warmed to ambient temperature for 30 minutes, heated at reflux for 5 hours, cooled, treated with 1N hydrochloric acid and concentrated. The concentrate was partitioned between ethyl acetate and brine, and the organic layer was washed with brine and water and concentrated. The concentrate was purified by flash chromatography with 50% ethyl acetate in hexane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09283222B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-21ad948c0b8e4a9facb190b2bce48c6e |
| Source note | uspto-grants-2016_03 |