HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-methylhydroxylamine hydrochloride → 6-bromo-2'-methyl-2-(tetrahydro-2H-pyran-3-yl)-2'H-spiro[chroman-4,5'-[1,2,4]oxadiazol]-3'-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-methylhydroxylamine hydrochloride | HCID 77906 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 178511922 | HCID 178511922 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 6-bromo-2'-methyl-2-(tetrahydro-2H-pyran-3-yl)-2'H-spiro[chroman-4,5'-[1,2,4]oxadiazol]-3'-amine | HCID 58423848 | 10% |
Reaction Steps
To a solution of methylhydroxylamine HCl salt (75 mg, 0.9 mmol) in anhydrous MeOH (10 mL) was added NaOMe (25 w % in MeOH, 0.13 mL), followed by (E)-N-(6-bromo-2-(tetrahydro-2H-pyran-3-yl)chroman-4-ylidene)cyanamide (300 mg, 0.9 mmol). After stirring for 10 min, the solvent was removed in vacuo. The residue was redissolved in DCM (20 mL). The mixture was filter, and the solvent was removed in vacuo. The resulting residue was purified by preparative TLC to give 20 mg of 6-bromo-2′-methyl-2-(tetrahydro-2H-pyran-3-yl)-2′H-spiro[chroman-4,5′-[1,2,4]oxadiazol]-3′-amine (50 mg, 10%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08921359B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-5c260bdb56714cc1950c96b199a14471 |
| Source note | uspto-grants-2014_12 |