HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 783358, compound → HCID 67234975, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 783358 | HCID 783358 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 67234975 | HCID 67234975 | 88.7% |
Reaction Steps
To a solution of 4-(5-chloro-2-nitrobenzyl)morpholine (5.1 g, 19.9 mmol) in HOAc (75 mL) is carefully added zinc dust (3.9 g, 59.6 mmol). After 2 h, the reaction is filtered through a bed of Celite and the filtrate is concentrated to remove most of the HOAc. The residue is then taken up in 2M aqueous K2CO3 and extracted with ethyl acetate. The organic layer is dried (Na2SO4) and concentrated to afford a brown oil. The crude material is partially purified by flash chromatography using a gradient of 0-5% methanol in CH2Cl2 to afford the title compound (4.0 g, 62%, 70% purity).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09150577B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-6223cf8e07e448fc92cf4e8fe12a7df2 |
| Source note | uspto-grants-2015_10 |