HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 131715644, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 131715643 | HCID 131715643 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 131715644 | HCID 131715644 | 97.5% |
Reaction Steps
The Boc-diester (I) (1.27 g, 2.36 mmol) was dissolved in dioxane (15 ml) and treated with 2.6 ml 1N sodium hydroxide solution at room temperature under argon for 4 hours. The reaction mixture was acidified (pH=2) with 3N hydrochloric acid and evaporated at reduced pressure. The residue was dissolved in ethyl acetate, washed with 3N hydrochloric acid, dried over MgSO4 and evaporated at reduced pressure. The residue was purified by flash chromatography (silica gel, 5% methanol/chloroform) to give 1.03 g of the title product: MS: MH+ =448); 1HNM (CDCl3): 7.33 (S, 5H), 5.07 (S, 2H), 5.20-4.80 (m, 1H), 4.42-4.05 (m, 1H), 2.32 (S, 2H), 1.43 (S, 9H) and 2.08-1.07 (m, 16H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04908475 |
| Source dataset | uspto-grants-1990_03 |
| ORD ID | ord-ffeb4928061a4511a9edc6799c64580a |
| Source note | uspto-grants-1990_03 |