HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 59215763, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 59215829 | HCID 59215829 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 59215763 | HCID 59215763 | 78.3% |
Reaction Steps
To a solution of (7S,9aS)-7-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)-8-(phenylmethyl)octahydropyrazino[2,1-c][1,4]oxazine (D126, 276 mg, 0.73 mmol) in MeOH (24 ml), cooled to 0° C., was added dropwise 12 N HCl (1.4 mL). The reaction mixture was stirred for 2 hrs at r.t., then it was put in the freezer for 12 hrs. The reaction mixture was warmed-up to r.t., further HCl was added (0.7 ml) and the reaction mixture was stirred for 2 more hrs. The mixture was filtered on a SCX cartridge washing with methanol and then with 2M methanolic ammonia. The fractions eluted with ammonia were combined and evaporated to dryness to give the title compound as a colourless oil (150 mg, y=78%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07919491B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-a88cc64f7ffa4ad5839a6a4a78857a28 |
| Source note | uspto-grants-2011_04 |