Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 25204456 | HCID 25204456 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 67431762 | HCID 67431762 | — |
Reaction Steps
180 mg of N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]-amino}propyl]-4-oxo-3-(1-propylbutyl)-3,4-dihydroquinazoline-8-carboxamide are dissolved in 2.5 cm3 of ethyl ether at a temperature close to 20° C. 0.53 cm3 of a 4M solution of hydrochloric acid in dioxane is added, while stirring and under argon, at a temperature of 5° C. The reaction mixture precipitates. The suspension is stirred for 10 min then the stirring is stopped in order to remove the supernatant. 5 cm3 of ethyl ether are again added. This operation is carried out 3 times. The last suspension is then concentrated under reduced pressure (5 kPa). 160 mg of N-[(1S,2R)-1-benzyl-2-hydroxy-3-{[3-(trifluoromethyl)benzyl]amino}propyl]-4-oxo-3-(1-propylbutyl)-3,4-dihydroquinazoline-8-carboxamide hydrochloride (1:1) are obtained in the form of a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08030320B2 |
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| Source dataset | uspto-grants-2011_10 |
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| ORD ID | ord-4c1cabff8e204faf98156ac08fe7152a |
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| Source note | uspto-grants-2011_10 |
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