Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 53744939 | HCID 53744939 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86743136 | HCID 86743136 | 85.7% |
Reaction Steps
Under an inert atmosphere, a solution of 1.7 g of the product of Example 5 in 400 ml of methanol was cooled to 0° C. and then over 15 minutes, 48 ml of 0.1N sodium hydroxide were added with stirring for 2 hours at 0° C. The reaction medium was neutralized with 5 ml of N hydrochloric acid, and the solvents were eliminated under reduced pressure at 30° C. The residual aqueous phase was extracted with methylene chloride and the combined organic phases were dried, and the solvents were eliminated under reduced pressure. After chromatography on silica (eluent:methylene chloride - methanol, 100-4), 1.30 g of the expected product melting at 142° C. were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04839358 |
|---|
| Source dataset | uspto-grants-1989_06 |
|---|
| ORD ID | ord-6930d2d6f3094e15b331ed22cd2b36bc |
|---|
| Source note | uspto-grants-1989_06 |
|---|