HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane → HCID 21914731, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Ethyl [4-(chloromethyl)-1,3-thiazol-2-yl]carbamate | HCID 21914836 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 21914731 | HCID 21914731 | 98.2% |
Reaction Steps
A mixed solution of ethyl 4-(chloromethyl)-1,3-thiazol-2-ylcarbamate (500 mg) in 1,4-dioxane (5 ml) and water (10 ml) was refluxed with stirring for 3.5 hours. After cooling, it was concentrated under reduced pressure. The mixture was partitioned between ethyl acetate and water. The organic phase was separated, washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (10 g) using a mixed solvent of hexane and ethyl acetate (2:1). The fractions containing the objective compound were collected and evaporated under reduced pressure to give colorless syrup (450 mg, 98.2%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07442715B2 |
| Source dataset | uspto-grants-2008_10 |
| ORD ID | ord-e711d4cf4c1b41f2aaaa89aa6168e0eb |
| Source note | uspto-grants-2008_10 |