Hydrochloric Acid → HCID 54344931, Verbindung

Temperatur

80 °C

Sodium thiomethoxide (8.64 g) and copper (I) oxide (8.79 g) were mixed with 2-bromo-4-iodophenol (XX, 14.72 g) in anhydrous DMF (100 mL). The mixture was stirred and heated at 80° C. for 48 h under nitrogen atmosphere. Then, the resultant slurry was treated with concentrated HCl (5 mL) and EtOAc (200 mL), and was filtered and rinsed with EtOAc (200 mL). The organic layers were partitioned with 1N HCl (150 mL), water (150 mL) and brine (150 mL) and dried over MgSO4, filtered and solvent removed in vacuo. Product was purified by silica gel column chromatography, the product eluted with dichloromethane/hexane (2:3), to give the desired product (5.22 g, 39%) as a light brown oil.

1. filtrationwas filtered
2. washrinsed with EtOAc (200 mL)
3. customThe organic layers were partitioned with 1N HCl (150 mL), water (150 mL) and brine (150 mL)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customsolvent removed in vacuo
7. customProduct was purified by silica gel column chromatography
8. washthe product eluted with dichloromethane/hexane (2:3)

ORD-Eintrag

ord-6b51951a3efd489a8ad3b1609431f221

Quelldatensatz

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08697720B2