HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → HCID 22623070, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 22622957 | HCID 22622957 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 22623070 | HCID 22623070 | 57.4% |
Reaction Steps
390 mg (1.603 mmol) of (±)-2-methyl-3-oxo-6-[(1-imidazolyl)-methyl]-3,4-dihydro-2H-1,4-benzoxazine is dissolved in 42 ml of dimethoxyethane, mixed with 1.297 g (3.206 mmol) of Lawesson's reagent and stirred for 46 hours at room temperature. After the solvent is spun in, the residue is chromatographed on silica gel (mobile solvent: methylene chloride/ethanol). The fractions that are obtained by chromatography are removed from the polar contaminants by shaking with saturated sodium bicarbonate solution. 238.5 mg (57%) of the desired product is isolated, ting point 206-210° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06365736B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-17d42d45e2fe4af3b8844cc1df0137d3 |
| Source note | uspto-grants-2002_04 |