HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 5-(N-(3-((N-(Biphenyl-4-ylmethyl)-3,5-dichloro-2-hydroxyphenylsulfonamido)methyl)benzyl)sulfamoyl)-2-methylbenzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 5-(Chlorosulfonyl)-2-methylbenzoic acid | HCID 308449 | — |
| Edukt | N-(3-(Aminomethyl)benzyl)-N-(biphenyl-4-ylmethyl)-3,5-dichloro-2-hydroxybenzenesulfonamide | HCID 58531388 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 5-(N-(3-((N-(Biphenyl-4-ylmethyl)-3,5-dichloro-2-hydroxyphenylsulfonamido)methyl)benzyl)sulfamoyl)-2-methylbenzoic acid | HCID 66616505 | 58,1% |
Reaktionsschritte
To a solution of N-(3-(aminomethyl)benzyl)-N-(biphenyl-4-ylmethyl)-3,5-dichloro-2-hydroxybenzenesulfonamide (50 mg, 0.095 mmol) and Et3N (0.13 mL) in CH2Cl2 (4 mL) was added a solid of 5-(chlorosulfonyl)-2-methylbenzoic acid (22.24 mg, 0.095 mmol) at rt and it was stirred at it for 70 min. Direct purification of the mixture after concentration by prep HPLC provided the desired product (40 mg, 58.1%) as a white solid after lyophilization. 1H NMR (CD3OD): δ 8.17 (d, J=2.0 Hz, 1H), 7.93 (dd, J=8.3, 2.2 Hz, 1H), 7.56˜6.90 (m, 15H), 6.76 (s, 1H), 4.34 (s, 2H), 4.31 (s, 2H), 3.87 (s, 2H), 2.52 (s, 3H); MS (ESI): (M+H)+=725.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08501992B2 |
| Quelldatensatz | uspto-grants-2013_08 |
| ORD ID | ord-70127a297d67473496f5e005ad3600ef |
| Quellennotiz | uspto-grants-2013_08 |