Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 21471606 | HCID 21471606 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 21471671 | HCID 21471671 | — |
Reaction Steps
The 1,3-dihydro-1-{1-[1-(2-tert-butoxycarbonylamino-5-pyrimidinylcarbonyl)piperidin-4-yl]piperidin-4-yl}-2H-benzimidazol-2-one was dissolved in ethyl acetate, cooled to -50° C. and treated with a stream of HCl gas for 2 min. The reaction mixture was allowed to warm to room temperature and stir for several hours, and then concentrated to dryness under reduced pressure. The product 1,3-dihydro-1-{1-[1-(2-amino-5-pyrimidinecarbonyl)piperidin-4-yl]piperidin-4-yl}-2H-benzimidazol-2-one dihydrochloride salt, was obtained as white solid: Analysis calculated for C22H25N7O2.2 HCl.1.0 C7H8.3.0 H2O: C: 54.38, H: 6.77, N: 15.31; found C: 54.31, H: 6.48, N: 15.23.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05691323 |
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| Source dataset | uspto-grants-1997_11 |
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| ORD ID | ord-a502673496e54607ad35e6d16061398d |
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| Source note | uspto-grants-1997_11 |
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