HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 69066344, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 69068852 | HCID 69068852 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 69066344 | HCID 69066344 | 14% |
Reaction Steps
0.25 g (0.53 mmol) of the product from Example 34 was dissolved in 15 ml of ethanol and 5 ml of 2N NaOH was added. The solution was heated to reflux for 3 hours, after which time it was concentrated then neutralized with 2N HCl. The mixture was extracted with ethyl acetate (2×20 ml) and the combined organic layers were dried (MgSO4) and concentrated. The crude solid was subjected to column chromatography on silica gel eluting with chloroform:methanol (95:5). The fractions containing product were combined and concentrated to yield a light tan solid, which was crystallized from ethyl acetate:hexane to yield 32 mg (14%) of product, mp 168-170° C. (d).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07563793B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-9613abbc23dc456d93152600130ac7bc |
| Source note | uspto-grants-2009_07 |