HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → HCID 67371284, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | HCID 11603852 | HCID 11603852 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67371284 | HCID 67371284 | 99% |
Reaction Steps
The title compound is prepared following the procedures of WO, 00 55159 as follows. A solution of 2-(3-nitropyridin-4-yl)malonic acid dibenzyl ester (1.58 g, 5.6 mmol), lithium chloride (250 mg, 10.6 mmol), dimethylsulfoxide (35 mL) and water (95 mL) is heated at reflux for 8 hr. After cooling to room temperature, the reaction is diluted with water and extracted with ethyl acetate. The combined extract is extracted with water, with brine, dried, filtered and concentrated to yield (3-nitropyridin-4-yl)acetic acid benzyl ester (1.13 g, 99% yield) as a yellow-orange oil. The material is purified by chromatography eluting with pentane-20 to 30% ethyl acetate to afford the product as a pink oil. MS 273 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07405300B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-26ec7b5193994dca8bbef23863d0b3c3 |
| Source note | uspto-grants-2008_07 |