HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68283667, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 71534205 | HCID 71534205 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 68283667 | HCID 68283667 | 61% |
Reaction Steps
To a solution of the compound obtained in Step D (261 mg, 0.86 mmol) in a mixture of methanol/water (2/0.2 mL) at ambient temperature there is added sodium hydroxide (86 mg, 2.14 mmol). The mixture is stirred for 1 hour under reflux, and the solution is then cooled. Hydrochloric acid (2.6 mL, 2.6 mmol, 1N) is added and the mixture is stirred overnight. The aqueous phase is extracted with dichloromethane, and the organic phases are washed with saturated NaCl solution, dried over magnesium sulphate, filtered and evaporated. The title compound is obtained after purification by flash column chromatography (ethyl acetate-petroleum ether: 90-10, then ethyl acetate-methanol: 90-10) in the form of an oil in a yield of 61%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08871975B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-f5ac5f1e37a04c4eae34493c9fbbb71d |
| Source note | uspto-grants-2014_10 |