Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Acetamidine monohydrochloride | HCID 67170 | — |
| Reactant | HCID 57855886 | HCID 57855886 | — |
| Product | HCID 57855962 | HCID 57855962 | 58% |
Reaction Steps
To a suspension of 1 g (3.48 mmol) of 2,5-diamino-3-chloro-4-methylamino-benzoic acid methyl ester (synthesis described in example H7) in 153 mL of EtOH is added 680 mg (6.97 mmol) of acetamidine hydrochloride. The mixture is stirred 2 days at a temperature of 80° C. Then, all the solvent is evaporated and the residue is suspended in EtOAc, the formed precipitate is filtrated and after evaporation the filtrate is purified by flash chromatography on silica gel and gave 510 mg (2.01 mmol, 58%) of a brown-reddish solid. LC/MS: 254/256 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08580785B2 |
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| Source dataset | uspto-grants-2013_11 |
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| ORD ID | ord-b4b44f2025aa4106b945a2ec16f1ae06 |
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| Source note | uspto-grants-2013_11 |
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