Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | 2-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide | HCID 66618074 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86691670 | HCID 86691670 | 96% |
Reaction Steps
Ethanol (29.3 ml) and water (0.74 ml) were added to 2-{4-amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide (1.034 g, 2.243 mmol), and the mixture was then stirred at 25° C. Thereafter, 2 M hydrochloric acid in ethanol (6.73 ml, 13.46 mmol) was added to the reaction mixture, and the resulting mixture was then stirred for 3 hours 45 minutes. Thereafter, the precipitated crystal was filtrated, was then washed with ethanol (5 ml), and was then dried under reduced pressure at 40° C. for 1 hour, so as to obtain the above title compound (1.118 g, 2.155 mmol). Yield: 96%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08815880B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-b99ab6992124479cac3b3dab0e16efe6 |
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| Source note | uspto-grants-2014_08 |
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