Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 18700091 | HCID 18700091 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 18700177 | HCID 18700177 | — |
Reaction Steps
Into a stirred solution of 1-(1-(2-(2,2,2-trifluoroethoxy)-4-(tert-butyloxycarbonylamino)phenylacetyl)piperidin-4-yl)-4H-3,1-benzoxazin-2(1H)-one (0.23 g, 0.41 mmol) from Step 10 above in EtOAc (75 mL) at 0° C. was bubbled HCl gas for 15 min. The resulting suspension was stirred at 0° C. for 45 min. Excess HCl was removed by bubbling argon though the mixture for 15 min. Ether (75 mL) was added and the cold suspension was filtered. The solids were washed with additional ether and dried under reduced pressure for 18 h to give the hydrochloride salt of the title compound as an amorphous white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06090805 |
|---|
| Source dataset | uspto-grants-2000_07 |
|---|
| ORD ID | ord-a4d29dd0898942c8b0a6963e81d79d3d |
|---|
| Source note | uspto-grants-2000_07 |
|---|