HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → Cyclopropanecarboxylic Acid 4-(3,6-dimethyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-2-methyl-benzylamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Cyclopropanecarbonyl chloride | HCID 77637 | — |
| Edukt | Riboflavin | HCID 493570 | — |
| Edukt | (4-Aminomethyl-3-methyl-phenyl)-(3,6-dimethyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulen-9-yl)-methanone | HCID 135736053 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | Cyclopropanecarboxylic Acid 4-(3,6-dimethyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-2-methyl-benzylamide | HCID 136128370 | 51% |
Reaktionsschritte
Triethylamine (0.145 ml, 1.04 mmol) and cyclopropanecarbonyl chloride (0.041 ml, 0.45 mmol) were added to a solution of (4-aminomethyl-3-methyl-phenyl)-(3,6-dimethyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulen-9-yl)-methanone from Example E101.2 (150 mg, 0.41 mmol) in dichloromethane (10 ml) at room temperature. The mixture was stirred for 20 h then concentrated in vacuo. The residue was purified by preparative HPLC (eluant; 0.5% 35% ammonia:9.5% methanol:90% dichloromethane) to give an off-white solid identified as the title compound (91 mg, 51%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08202858B2 |
| Quelldatensatz | uspto-grants-2012_06 |
| ORD ID | ord-59d695f6394449a0a66d327c81572566 |
| Quellennotiz | uspto-grants-2012_06 |