HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 10299722, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 86587864 | HCID 86587864 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Sodium Methoxide | HCID 10942334 | — |
| Product | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 10299722 | HCID 10299722 | 37% |
Reaction Steps
Methyl (5R,7S,8R)-8-{[4-(1,1-dioxido-3,4-dihydro-2H-1-benzothiopyran-4-yl)benzoyl]amino}-1-oxaspiro[4.4]nonane-7-carboxylate from reaction 33f (0.165 mmol) was dissolved in a solution of hydroxylamine hydrochloride, methanol and sodium methoxide, (2 mL) under nitrogen atmosphere at room temperature. The reaction was stirred for 1 h, made neutral with TFA, concentrated and purified by HPLC on a C-18 column eluting with an acetonitrile:water:TFA gradient, to give the title compound (0.03 g, 37%) as a white solid. MS found: (M+H)+=485, (2M+H)+=969.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06720329B2 |
| Source dataset | uspto-grants-2004_04 |
| ORD ID | ord-f81a0ca685ee451c81363e6240cdefd3 |
| Source note | uspto-grants-2004_04 |