Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethoxyacetyl chloride | HCID 84189 | — |
| Reactant | 2-Chloro-N4-(2-methylpropyl)-6-methylpyridin-3,4-diamine | HCID 22715003 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22715001 | HCID 22715001 | — |
Reaction Steps
Anhydrous dichloromethane (750 ml) and 2-chloro-N4-(2-methylpropyl)-6-methylpyridin-3,4-diamine (18.84 g) were combined and cooled to 0° C. Triethylamine (12.9 ml) was added dropwise to the resulting mixture, and then ethoxyacetyl chloride (11.34 g) dissolved in anhydrous dichloromethane (50 ml) was added slowly to the resulting mixture, which turned dark. After two hours the dark mixture was allowed to warm to room temperature. TLC analysis of the reaction mixture indicated completion, and the solvent was removed under reduced pressure. The resulting yellow solid was dissolved in chloroform, and the resulting solution was washed with water. The organic layer was dried with magnesium sulfate and concentrated to a dark brown oil (27.75 g) under reduced pressure. NMR analysis of the oil indicated desired product of suitable purity for use in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06743920B2 |
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| Source dataset | uspto-grants-2004_06 |
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| ORD ID | ord-ca1589a51e0d4996bf9068ed833c9673 |
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| Source note | uspto-grants-2004_06 |
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