Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyanuric chloride | HCID 7954 | — |
| Reactant | 4-Amino-2-chlorophenol | HCID 77578 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 21897019 | HCID 21897019 | 99% |
Reaction Steps
Cyanuric chloride (12.95 g, 70.0 mmol) was dissolved in acetone (200 mL), the solution was cooled to 0-5° C. with an ice bath, and 4-amino-2-chlorophenol (10.09 g, 70.0 mmol) in acetone (100 mL) was added. The mixture was stirred at 0-5° C. for 1 hour under nitrogen. The reaction mixture was extracted three times using dichloromethane; the combined organic layer were washed with brine and dried over sodium sulfate. The sample was concentrated in vacuo, and the resulting solid was dried overnight under vacuum to yield E6 (20.2 g, 99%); mp 180° C.; HPLC: Inertsil ODS 3V C18, 40:30:30 v:v:v [KH2PO4 (0.01 M, pH 3.2):CH3OH:CH3CN], 264 nm, Rt 11.6 min, 99.4% purity; MS (TOF ES+) m/z 293 (97.5), 291 (M+H, 100).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07112587B2 |
|---|
| Source dataset | uspto-grants-2006_09 |
|---|
| ORD ID | ord-4901bf8576d84f1599616213981c2f7f |
|---|
| Source note | uspto-grants-2006_09 |
|---|