HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69953870, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 69953686 | HCID 69953686 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 69953870 | HCID 69953870 | 78.5% |
Reaction Steps
Intermediate 1B (320 mg, 1.2 mmol) was treated with 1.31 ml of 1 N NaOH, a small amount of MeOH was added to aid dissolution of the ester. The resulting suspension was stirred for 2 h then acidified with 1N HCl and EtOAc was added. The organic layer was separated, washed with brine, dried over Na2SO4 then filtered and the solvent removed to yield 240 mg oil. The crude product was purified by reverse phase preparative HPLC (C18, MeOH/H2O (0.1% TFA)-gradient). MS (M−H) calcd for C12H10NO4Cl: 253.0268; found: 253.0267.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06548546B2 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-230541a0d2da482b8ba3cab191173754 |
| Source note | uspto-grants-2003_04 |