HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 67365120, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | HCID 5179950 | HCID 5179950 | — |
| Reactant | HCID 72751052 | HCID 72751052 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 67365120 | HCID 67365120 | — |
Reaction Steps
To a solution of 4-chloro-5,5,5-trifluoro-3-phenylpent-3-en-2-one (950 mg) and methylsulfanylacetate (446 mg) in MeCN (23.8 mL) was added dropwise DBU (0.63 mL) at 25° C., followed by stirring at the same temperature for 15 hours. To the reaction liquid was added a saturated aqueous NH4Cl solution (50 mL), followed by extraction with diethylether (50 mL) three times. The organic layer was washed with brine, dried over MgSO4, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=98:2 to 90:0) to obtain methyl 3-methyl-4-phenyl-5-(trifluoromethyl)thiophene-2-carboxylate (1.08 g) as a colorless liquid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08193378B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-666ff529af1e44bbb3a58508ab6692cc |
| Source note | uspto-grants-2012_06 |