Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | HCID 86633782 | HCID 86633782 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 86633781 | HCID 86633781 | 115.2% |
Reaction Steps
To a slurry of 7-(4-methoxy-phenyl)-isoquinoline-5-sulfonic acid (12.13 g, 38.5 mmol) in 1,2-dichloroethane (200 mL) and DMF (2.99 mL, 38.5 mmol) add oxalyl chloride (26.8 mL, 308 mmol) dropwise. Mechanically stir the slurry under nitrogen atmosphere while heating at 60-65° C. for 4 hr. Cool the slurry to −10° C. Wait for 30 min then filter. Wash the yellow solid with 20% ether/dichloromethane and dry under a nitrogen atmosphere affording the title compound (14.8 g) as a yellow powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07998977B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-4ca403d36c874b9698c4e07e1ad53c26 |
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| Source note | uspto-grants-2011_08 |
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