HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → HCID 86741128, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 13749130 | HCID 13749130 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 86741128 | HCID 86741128 | 98.2% |
Reaction Steps
A solution of 6,7,8,9-tetrahydro-3-methoxy-10-methylpyrido[1,2-a]indol-9-one (2.29 g, 10 mmol) and hydroxylamine hydrochloride (1.39 g, 20 mmol) in dry pyridine (40 mL) was refluxed for 2 hours. The reaction mixture was concentrated to 10% of its original volume and distilled water (80 mL) was added. The organic product was extracted with ether (3×60 mL). The combined organic layers were washed with water (100 mL), 5% hydrochloric acid (50 mL), and 10% sodium bicarbonate (50 mL). The separated organic layer was dried over MgSO4, filtered, and evaporated. The residue was recrystallized from methanol/water to afford 2.4 g (98%) of the title compound as gray microcrystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04624954 |
| Source dataset | uspto-grants-1986_11 |
| ORD ID | ord-b6694d89f6844b22b724ccdd1faaeef7 |
| Source note | uspto-grants-1986_11 |