Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 67452116 | HCID 67452116 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 67451921 | HCID 67451921 | — |
Reaction Steps
2.5 g ((2-(2-(2-(Bis-methoxycarbonylmethyl-amino)-phenoxy)-ethoxy)-4-fluoro-phenyl)-methoxycabonylmethyl-amino)-acetic acid methyl ester were dissolved in 30 ml glacial acetic acid. Under vigorous stirring 4.54 ml 1 molar nitric acid in glacial acetic acid was added and in a second step 11.35 ml of concentrated sulfuric acid was added. The temperature increased up to 30° C. The reaction mixture was directly poured in a 250 ml ice/water mixture. The residue was filtered off, washed several times with water and dried under vacuum. The crude product was further purified by column chromatography on silica gel first with hexane/acetic acid ethyl ester (1:1) as eluent and a second time with toluene/acetonitrile (1:1) as eluent. Yield: 0.82 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08962338B2 |
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| Source dataset | uspto-grants-2015_02 |
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| ORD ID | ord-d56bb863645a4a45973330f6dbe2cb7f |
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| Source note | uspto-grants-2015_02 |
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