Dimethylformamide → HCID 86656259, Verbindung

A suspension of 3-(2′,4′-dichlorobiphenyl-4-ylsulfonamido)benzoic acid (1.50 g, 3.56 mmol) in DCM (35 mL) was stirred at 0° C. and oxalyl chloride (340 μL, 3.9 mmol) was added, followed by a catalytic amount of DMF (<50 μL). The mixture was allowed to warm to room temperature and stirred for two days, during which time the solid dissolved to form a light yellow clear solution. The mixture was evaporated under reduced pressure and the residue was azeotroped with toluene (3 mL), then hexane (10 mL) and the title compound obtained as a light brown, slightly gummy, solid (1.5 g) which was used without further purification.

1. temperatureto warm to room temperature
2. stirringstirred for two days, during which time the solid
3. dissolutiondissolved
4. customto form a light yellow clear solution
5. customThe mixture was evaporated under reduced pressure
6. customthe residue was azeotroped with toluene (3 mL)

ORD-Eintrag

ord-5a21c4556dd8419cb5b4b454fde0a520

Quelldatensatz

uspto-grants-2012_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08207167B2