Participants
| Role | Name | HCID | Charge |
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| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 71240780 | HCID 71240780 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 71244917 | HCID 71244917 | 98% |
Reaction Steps
4M HCl in dioxane solution (8 ml) was added in one portion to a stirred solution of 4-[6-(3,4-Dichloro-phenyl)-pyrimidin-4-yl]-piperazine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (0.36 g, 0.75 mmol) in dioxane (2 ml) and the mixture was stirred at room temperature overnight. After this time the reaction mixture was concentrated and the resulting residue was partitioned between DCM (100 ml) and saturated sodium bicarbonate (75 ml) and stirred at room temperature for 10 minutes. The mixture was then extracted with DCM (3×100 ml), the organic layers were combined, separated and washed with brine (50 ml). The organic layer was removed, dried (MgSO4) filtered and concentrated to give the title compound (0.27 g, 87% yield) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09260422B2 |
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| Source dataset | uspto-grants-2016_02 |
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| ORD ID | ord-b9ba49df27e542ae9477436c7a321bb6 |
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| Source note | uspto-grants-2016_02 |
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