HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9858633, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Cyanuric chloride | HCID 7954 | — |
| Reactant | HCID 21083990 | HCID 21083990 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 9858633 | HCID 9858633 | 71.1% |
Reaction Steps
A mixture of cyanuric chloride (28 mg, 0.15 mmol) and the compound of Example 75 (52 mg, 0.15 mmol) in DMF (1.5 mL) was heated at 110° for 18 h. Two further portions of cyanuric chloride (14 mg, 0.075 mmol) were added and heating continued for a further 26 h. Water was added and the precipitate filtered off, washed with water and dried. The crude product was purified by column chromatography on silica (1% THF in DCM) to give the title compound as a white solid (35 mg, 71%). δH (DMSO-d6) 7.78 (1H, d, J 9.6 Hz), 7.71–7.67 (1H, m), 7.66–7.64 (1H, m), 7.64–7.59 (7H, m), 7.59–7.58 (1H, m), 6.67 (1H, d, J 9.6 Hz). LCMS (ES+) RT 3.65 minutes, 329 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176215B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-a59307fadada455d8092571db613b032 |
| Source note | uspto-grants-2007_02 |