HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 59003222, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 59003133 | HCID 59003133 | — |
| Product | HCID 59003222 | HCID 59003222 | 96% |
Reaction Steps
Add 2 N sodium hydroxide solution (2 mL) to a solution of isopropyl-5-[acetyl-(3,5-bistrifluoromethylbenzyl)amino]-7-bromo-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (0.100 g, 0.174 mmol) in methanol (5 mL) at 0° C. and allow to stir for 30 min. Acidify to pH 4 with 2 N hydrochloric acid solution and extract the aqueous mixture with ethyl acetate (3×10 mL). Wash the organic layer with water and brine (10 mL each). Dry the organic layer over anhydrous sodium sulfate, filter and remove the solvent under reduced pressure. Purify the residue by triturating with water, to provide the title compound as a white solid (0.091 g, 96%): APCI MS 561 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07749992B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-16f8a987321a47bea8fc57e485caaafd |
| Source note | uspto-grants-2010_07 |