Participants
| Role | Name | HCID | Charge |
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| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 68834385 | HCID 68834385 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 57642205 | HCID 57642205 | 91% |
Reaction Steps
4.0M HCl in dioxan (5 ml, 20.0 mmol) was added to a solution of (3-{2-[5-cyclohexyl-1-(3,3-dimethyl-2-oxo-butyl)-2-oxo-1,2-dihydro-3H-1,3,4-benzotriazepin-3-yl]-acetylamino}-phenyl)-propyl-carbamic acid tert-butyl ester (Example 41, step a) (524 mg, 0.83 mmol) in dioxan (15 ml) at room temperature. The mixture was stirred for 2 h during which time a white precipitate formed. The solvent was evaporated, and the solid obtained was washed with Et2O, isolated by filtration and dried, to afford the hydrochloride salt of the title compound (430 mg, 91%). 1H NMR (CDCl3) 8.39 (1H, s), 7.61-7.27 (7H, m), 7.01 (1H, d), 4.69 (2H, br s), 4.60 (1H, d), 4.29 (2H, dd), 3.21 (2H, br s), 2.80 (1H, br s), 2.01-1.45 (6H, m), 1.43-1.19 (15H, m), 0.95 (3H, t). Found: C, 63.68; H, 7.65; N, 11.98%; C31H41N5O3.HCl.H2O requires: C, 63.52; H, 7.57; N, 11.95%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07524837B2 |
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| Source dataset | uspto-grants-2009_04 |
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| ORD ID | ord-ce4c1d1db690405daec9b9c9c5143c78 |
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| Source note | uspto-grants-2009_04 |
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