HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4-(4-chloro-phenyl)-7,8-dimethoxy-4H-1,3,4-triaza-phenalene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 7,8-dimethoxy-4-(4-chloro-phenyl)-5,6-dihydro-4H-1,3,4-triaza-phenalen-5-ol | HCID 21098405 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-(4-chloro-phenyl)-7,8-dimethoxy-4H-1,3,4-triaza-phenalene | HCID 11772159 | — |
Reaction Steps
To a solution of 7,8-dimethoxy-4-(4-chloro-phenyl)-5,6-dihydro-4H-1,3,4-triaza-phenalen-5-ol (140 mg, 0.39 mmol) (from Example 21, Step A, supra) and triethylamine (0.32 mL, 2.33 mmol) in dichloromethane (50 mL) at 0° C. was added methanesulfonyl chloride (0.12 mL, 1.55 mmol) (Aldrich). The reaction solution was the stirred at room temperature for 2 hours. The solution was then concentrated, the residue was purified by chromatography using EtOAc/CH2Cl2/NEt3 (1:1:0.01) as eluent to give the desired 4-(4-chloro-phenyl)-7,8-dimethoxy-4H-1,3,4-triaza-phenalene as a yellow solid. (Yield 47 mg, 55%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07217717B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-284bfd0f28634ab8b060fe60adf3f5b2 |
| Source note | uspto-grants-2007_05 |