Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Sulfamide | HCID 82267 | — |
| Reactant | HCID 66614166 | HCID 66614166 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66635554 | HCID 66635554 | — |
Reaction Steps
550 mg (1.093 mmol) of the compound from example 92A were divided between 11 microwave vessels. 50 mg of the substance in each were admixed with 48 mg (0.496 mmol) of sulfamide and 2.5 ml of pyridine and then heated at 160° C. under microwave radiation for 30 min. Subsequently, all batches were combined and freed of the solvent under reduced pressure. The residue was taken up in dichloromethane and extracted three times with water. The phases were separated and the organic phase was dried with sodium sulfate, filtered and concentrated under reduced pressure. The residue was then purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient). This gave 0.130 g (12% of theory, purity 50%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09096592B2 |
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| Source dataset | uspto-grants-2015_08 |
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| ORD ID | ord-0bf5ac7f67f44938a149355ffc6439a6 |
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| Source note | uspto-grants-2015_08 |
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