HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → HCID 71585443, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 89602064 | HCID 89602064 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 71585443 | HCID 71585443 | 38.7% |
Reaction Steps
To a solution of methyl 4-((2-methyl-1-oxo-1,2,3,4-tetrahydropyrazino[1,2-a]indol-10-yl)thio)benzoate (0.25 g, impure) and NH2OH.HCl (0.35 g) in 4 mL of dry MeOH was added 1.4 mL of 25% NaOMe solution in methanol. The reaction mixture was stirred for 20 min at r.t. and 0.3 mL of more 25% NaOMe solution in methanol was added. After stirring for 2 h, the reaction mixture was quenched with 10 mL of potassium phosphate buffer solution. The mixture was extracted with 2×30 mL of EtOAc. The combined extracts were dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel chromatography eluted with up to 10% MeOH/CH2Cl2 to give 0.097 g of the title product as beige solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09345905B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-7936f437a3504f6d9dec5d40af11327c |
| Source note | uspto-grants-2016_05 |