Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 68638028 | HCID 68638028 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68638699 | HCID 68638699 | 82% |
Reaction Steps
To a stirred solution of {4-[3-tert-butoxycarbonylamino-4-(2,4,5-trifluoro-phenyl)-butyryl]-2-oxo-2,3,4,5-tetrahydro-benzo[e][1,4]diazepin-1-yl}-acetic acid methyl ester (90 mg, 0.16 mmol) in THF (2 mL) and water (2 mL), was added lithium hydroxide (40 mg, 0.95 mmol). The reaction mixture was stirred at r.t. overnight. After the completion of the reaction as confirmed by TLC, the reaction mixture was cooled to 0° C. and neutralized with 10% HCl solution and the pH was adjusted to 1. The crude compound was extracted with ethylacetate (10 mL). The organic layer was washed with water, dried over Na2SO4. The solvents were removed in vacuo to afford {4-[3-tert-butoxycarbonylamino-4-(2,4,5-trifluoro-phenyl)-butyryl]-2-oxo-2,3,4,5-tetrahydro-benzo[e][1,4]diazepin-1-yl}-acetic acid (70 mg, 82%) as a viscous oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08455479B2 |
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| Source dataset | uspto-grants-2013_06 |
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| ORD ID | ord-933a5a2855414b9cbbe975639745e717 |
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| Source note | uspto-grants-2013_06 |
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