HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 69655194, compound → HCID 21936925, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 69655194 | HCID 69655194 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 21936925 | HCID 21936925 | 65.6% |
Reaction Steps
A suspension of 0.7 g of (±)-1-methoxy-5-oxo-6,7,8,9-tetrahydro-5H-benzocycloheptene-7-carboxylic acid ethyl ester (prepared as described in Bowman, Tetrahedron, 48, 4027, 1992) in 2 mL of 2N NaOH was refluxed for 2 h, then cooled and extracted with Et2O. The aqueous layer was brought to acidic pH with 10% HCl, the precipitate formed was redissolved in Et2O and the organic phase was washed with water and dried. The solvent was removed in vacuo and the resulting residue was purified by flash chromatography, eluting with a mixture CH2Cl2/MeOH 9:1 respectively, yielding 0.41 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115633B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-93e075eda2c94946a3583a0558b651c2 |
| Source note | uspto-grants-2006_10 |