HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → HCID 59177867, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Methyl 3-(3,5-dichloropyridin-2-yl)-2-(2-fluorophenyl)-3-oxopropanoate | HCID 59177868 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59177867 | HCID 59177867 | — |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
A mixture of 4.50 g (13.2 mmol) of methyl 3-(3,5-dichloropyridin-2-yl)-2-(2-fluorophenyl)-3-oxopropanoate from example 1A, 845 mg (14.5 mmol) of sodium chloride, 474 mg (26.3 mmol) of water and 13.5 ml of DMSO is heated in a microwave at 150° C. for 10 min and then stirred into water and extracted with ethyl acetate. The organic phase is dried over sodium sulfate and concentrated. The residue is purified by chromatography on silica gel (eluent: dichloromethane) to result in a yellow oil which gradually crystallizes and affords 3.18 g (85% of theory) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08309551B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-191caca329264534bddcfb489060d957 |
| Source note | uspto-grants-2012_11 |