HuagongsheHuagongshe Chemistry Print Report · For research reference only
O-Methylhydroxylamine hydrochloride → HCID 86707895, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | HCID 68291126 | HCID 68291126 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 86707895 | HCID 86707895 | 95.2% |
Reaction Steps
A solution of 1-benzyl 3-methyl 4-oxopyrrolidine-1,3-dicarboxylate (12 g, 43.2 mmol) in pyridine (50 mL) at 0° C. was added O-methylhydroxylamine hydrochloride (5.51 g, 66.0 mmol) which was stirred for 10 minutes, and then it was warmed up to RT and stirred for 16 hrs. The reaction mixture was concentrated to yield a crude product which was partitioned in 300 mL of 1N HCl and 300 mL of EtOAc. The organic layer was washed with 100 mL of brine. The combined aqueous phases were extracted with 200 mL of EtOAc. The combined organic phases were dried over Na2SO4. Filtration and concentration to yield the product (12.6 g, 95% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09428511B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-acb6638ba12e47b4a5f280f4423ef373 |
| Source note | uspto-grants-2016_08 |