HuagongsheHuagongshe Chemistry Print Report · For research reference only
(4-Nitrophenoxy)-acetic acid methoxycarbonylmethyl ester → HCID 59253947, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (4-Nitrophenoxy)-acetic acid methoxycarbonylmethyl ester | HCID 59253951 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59253947 | HCID 59253947 | 73.1% |
Reaction Steps
(4-Nitrophenoxy)-acetic acid methoxycarbonyl methyl ester 44 (20 g, 74.3 mmol) was dissolved in dimethyl formamide (100 ml) in a pressure vessel. Palladium on carbon (5%, 8 g) was added, and the mixture stirred under an atmosphere of hydrogen (4 kg) for 2 hours. The catalyst was removed by filtration and ice water (400 ml) was added to the filtrate. Crude 45 was extracted into ethyl acetate, dried over Na2SO4 and distilled. Crude 45 was then recrystallised from chloroform:hexane (1:6) to get pure 45 (13 g, 73%) as a light brown shining powder with an m.p. between 76.5-78.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846845B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-ab71e9edf5b5472c9a02a544801083ef |
| Source note | uspto-grants-2014_09 |