HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 5-(3-Bromophenyl)-5-methyl-3-morpholinethione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | 5-(3-Bromophenyl)-5-methylmorpholin-3-one | HCID 58155305 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-(3-Bromophenyl)-5-methyl-3-morpholinethione | HCID 72681267 | — |
Reaction Steps
A solution of 5-(3-bromo-phenyl)-5-methyl-morpholin-3-one (18 g, 67 mmol) in dry THF was treated with Lawesson's reagent (27 g, 67 mmol) in one portion at room temperature. The mixture was refluxed for 2 h. The title compound was obtained by chromatography on silica gel (PE/EtOAc=30:1 to 10:1). 1H-NMR (400 MHz, DMSO-d6): 11.08 (s, 1H), 7.50 (m, 2H), 7.35 (m, 2H), 4.36 (s, 2H), 4.00 (m, 1H), 3.73 (m, 1H), 1.51 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08207164B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-75714e20b5784b4592c839bae3b40675 |
| Source note | uspto-grants-2012_06 |