1-Hydroxybenzotriazole → HCID 10296065, Verbindung

2′-Methyl-5′-(5-methyl-1,3,4-oxadiazol-2-yl)-1,1′-biphenyl-4-carboxylic acid (11.3 mg, 0.034 mmol), HOBT (6.0 mg, 0.044 mmol), 1-(3-dimethylaminopropyl)-3-ethyl carbodiimide hydrochloride (8.0 mg, 0.042 mmol) and 3-dimethylaminobenzylamine (0.34 mmol) were mixed in DMF (0.7 ml) and the reaction left at room temperature for 18 h. The DMF was evaporated under vacuum and the residue partitioned between DCM (0.4 ml) and water (0.4 ml). The organic phase was washed with aqueous sodium hydroxide (0.5M, 0.2 ml) and the DCM evaporated under vacuum. The residue was purified by mass directed HPLC to give N-(3-dimethylaminobenzyl)-2′-methyl-5′-(5-methyl-1,3,4-oxadiazol-2-yl)-1,1′-biphenyl-4-carboxamide. LCMS; retention time 3.11 min, MH+ 427.

1. customThe DMF was evaporated under vacuum
2. customthe residue partitioned between DCM (0.4 ml) and water (0.4 ml)
3. washThe organic phase was washed with aqueous sodium hydroxide (0.5M, 0.2 ml)
4. customthe DCM evaporated under vacuum
5. customThe residue was purified by mass

ORD-Eintrag

ord-5044537486624900aeae3ca0bb436221

Quelldatensatz

uspto-grants-2008_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07384963B2