HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 19883554, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 21835134 | HCID 21835134 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 19883554 | HCID 19883554 | 72.1% |
Reaction Steps
To a solution of 0.26 g (1.5 mmol) of ethyl 2-(1,3-thiazol-2-yl)propanoate from step A above in 15 mL of methanol was added 3.0 mL (15 mmol) of an aqueous 5.0 M sodium hydroxide solution. The resulting mixture was stirred at ambient temperature overnight. The reaction mixture was evaporated in vacuo to remove the methanol and the aqueous phase was acidified with a 2 N hydrochloric acid solution until a pH of 4 was achieved. The aqueous solution was purified by reverse phase HPLC (TMC Pro-Pac C18; 0-25% 0.1% trifluoroacetic acid in acetonitrile/0.1% trifluoroacetic acid in water gradient). The pure fractions were lyophilized overnight to afford the title compound as a white solid (0.17 g, 71%). LC-MS: m/z (ES) 158 (MH)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399480B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-6eb148a8bf08450289ca3091390fd1e8 |
| Source note | uspto-grants-2013_03 |