HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 117974095, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethanethiol | HCID 6343 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 117974122 | HCID 117974122 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 117974095 | HCID 117974095 | — |
Reaction Steps
0.31 g of sodium hydride (60%) was added to 20 ml of a solution of 2.76 g of 2-(3-bromothiophen-2-yl)-5-(trifluoromethylthio)benzoxazole and 0.6 ml of ethanethiol in NMP at 0° C., and the mixture was stirred at room temperature for 1 hour. Water was poured into the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with a 10% aqueous hydrochloric acid solution and a saturated aqueous salt solution and dried over anhydrous sodium sulfate, then concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 2.65 g of 2-(3-ethylthiothiophen-2-yl)-5-(trifluoromethylthio)benzoxazole (Compound of Present Invention (30)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09120792B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-282fcbbdfedc49f0b290375a6e30f0f8 |
| Source note | uspto-grants-2015_09 |