Potassium Carbonate → HCID 72326549, Verbindung

Temperatur

100 °C

A Schlenk tube was charged with 4,4′-dibromobenzil (1.8 g, 4.9 mmol), K2CO3 (3.38 g, 24.5 mmol), Bu4NBr (1.58 g, 4.9 mmol), LiCl (0.21 g, 4.9 mmol), Pd(OAc)2 (0.11 g, 0.49 mmol), 1,2-bis-dodecyloxy-4-vinyl-benzene (JYC-II-004-A) (5.78 g, 12.2 mmol), and 40 mL of dry DMF. The reaction mixture was heated at 100° C. under Ar over the weekend. The reaction mixture was allowed to cool down to room temperature and extracted with CH2Cl2. The organic phase was washed with H2O and dried over anhydrous MgSO4. The solvent was removed under reduced pressure. The crude product was purified by column chromatography (silica gel, dichloromethane:hexanes=1:2 (v/v), dichloromethane:hexanes=1:1 (v/v)), then dichloromethane:hexanes=3:2 (v/v)) to give a bright yellow solid. The solid was further recrystallized from CH2Cl2/hexanes to give a bright yellow solid (4.27 g, 75.6%).

1. temperatureto cool down to room temperature
2. extractionextracted with CH2Cl2
3. washThe organic phase was washed with H2O
4. dry with materialdried over anhydrous MgSO4
5. customThe solvent was removed under reduced pressure
6. customThe crude product was purified by column chromatography (silica gel, dichloromethane:hexanes=1:2 (v/v), dichloromethane:hexanes=1:1 (v/v))
7. customdichloromethane:hexanes=3:2 (v/v)) to give a bright yellow solid
8. customThe solid was further recrystallized from CH2Cl2/hexanes

ORD-Eintrag

ord-e20a54ff28364db7b40e488c40ecf21a

Quelldatensatz

uspto-grants-2010_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07842830B2