Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Amino-4,6-dichloropyrimidine | HCID 65522 | — |
| Reactant | HCID 59305024 | HCID 59305024 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 11682846 | HCID 11682846 | — |
Reaction Steps
57 mg (210 mmol) of N1-(3-chloro-1H-pyrrolo[2,3-b]pyridin-4-yl)-2-fluorobenzene-1,4-diamine and 47 mg (290 μmol) of 4,6-dichloropyrimidine-2-amine are suspended in 5 ml of water. 290 μl (290 mmol) of 1 M hydrochloric acid are added, and the mixture is stirred at 100° C. overnight. Using 1N aqueous sodium hydroxide solution, the suspension is then adjusted to pH 10, resulting in the precipitation of crystals. The solid is filtered off and washed with water. The crude product is purified by column chromatography on silica gel (mobile phase: dichloromethane/methanol (7M ammonia) 100:1 to 10:1) and subsequent preparative RP-HPLC.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07723347B2 |
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| Source dataset | uspto-grants-2010_05 |
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| ORD ID | ord-b6127d2476354fc199f20c36e8071d1d |
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| Source note | uspto-grants-2010_05 |
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