Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 131733550 | HCID 131733550 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 89644203 | HCID 89644203 | — |
Reaction Steps
The ethyl (2R)-2-[(3S)-3-(2-(dimethylamino)thiazol-5-ylsulphonylamino)-2-oxopyrrolidin-1-yl]-3-(7-methoxy-1-(tritylamino)isoquinolin-6-yl)propanoate obtained above (0.35 g, 0.44 mmol) is dissolved in 5 ml of dichloromethane. The medium is cooled to 0° C. and 0.5 ml of a 4N solution of hydrochloric acid in dioxane is added. The medium is stirred at 20° C. for 18 h. It is concentrated to dryness and the residue is triturated from ether and filtered off. It is purified on a column of silica (40 g, gradient CH2Cl2/MeOH/NH4OH; 100:0 to 90:10:0.5). The product thus obtained is dissolved in 5 ml of dichloromethane and salified with 0.5 ml of a 4N solution of hydrochloric acid in dioxane. The medium is concentrated and the residue is triturated from ether and dried over P2O5. 230 mg of a solid are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09150544B2 |
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| Source dataset | uspto-grants-2015_10 |
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| ORD ID | ord-1bf722bef72a4c1ead4bf306631403e6 |
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| Source note | uspto-grants-2015_10 |
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