HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → Thiazole, 5-methyl-2-(trifluoromethyl)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | Trifluoroacetamidoacetone | HCID 14076243 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | Thiazole, 5-methyl-2-(trifluoromethyl)- | HCID 15239222 | — |
Reaction Steps
Trifluoroacetamidoacetone (8.45 g, 50 mmol) and 20.2 g (50 mmol) of Lawesson's reagent were slurried in 100 mL of benzene and the mixture heated at reflux with stirring for 4-5 hr to obtain a clear solution. This was allowed to cool and was washed with 50 mL of 10 percent aqueous sodium hydroxide solution, dried over magnesium sulfate, and filtered. The resulting solution was kugelrohr distilled at 160° C. and the distillate was distilled through a 40 cm column packed with glass helices (to remove the benzene) until the head temperature began to drop. It was then distilled through a 20 cm Vigreauz column to obtain 5.1 g (61 percent of theory) of the title compound as a pale oil boiling at 138°-141° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05324837 |
| Source dataset | uspto-grants-1994_06 |
| ORD ID | ord-11e7f7b9018d4c78bd80d87860352fa5 |
| Source note | uspto-grants-1994_06 |