Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 178504606 | HCID 178504606 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178504584 | HCID 178504584 | — |
Reaction Steps
324 mg of (RS)-5-bromo-2-[4-(methylsulfinyl)phenylamino]pyrimidin-4-ol and 128 mg of sodium azide are suspended in 6 ml of methylene chloride and mixed drop by drop with 0.3 ml of concentrated sulfuric acid while being cooled with ice. The mixture is stirred for 36 hours at 40° C. The organic phase is decanted off, and the residue is stirred with ice water. The solid is suctioned off, washed twice with water and once with ethanol and dried. 266 mg (78.2% of theory) of the product with a melting point of 230° C. (decomposition) is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08507510B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-b4c268d8ccae4d1b86c7b359d8813558 |
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| Source note | uspto-grants-2013_08 |
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