Ethanol → 6-Hydroxy-2-(4-hydroxyphenyl)-3-(4-(2-piperidinoethoxy)-benzoyl]benzo[b]thiophene Hydrochloride 1,2-Dichloroethane

Temperatur

35 °C

A solution of 6-methoxy-2-(4-methoxyphenyl)-3-[4-(2-piperidinoethoxy)benzoyl]benzo[b]thiophene hydrochloride (2.0 g) in 1,2-dichloroethane (20 mL) was treated with boron trichloride (2.0 mL). The resulting mixture was stirred at 35° C. for about 18 hours. A mixture of ethanol and methanol (10 mL, 95:5, 3A) was treated with the reaction mixture from above, causing the alcoholic mixture to reflux. Upon complete addition, the resulting crystalline slurry was stirred at 25° C. After one hour, the crystalline product was filtered, washed with cold ethanol (10 mL), and dried at 40° C. in vacuo to give 1.78 g of the title compound. The X-ray powder diffraction pattern is identical to that reported in Table 1.

1. additionwas treated with the reaction mixture from above,
2. temperatureto reflux
3. additionUpon complete addition
4. stirringthe resulting crystalline slurry was stirred at 25° C
5. waitAfter one hour
6. filtrationthe crystalline product was filtered
7. washwashed with cold ethanol (10 mL)
8. customdried at 40° C. in vacuo

ORD-Eintrag

ord-e8ea92b8528041f484958dbcbab02358

Quelldatensatz

uspto-grants-2002_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06458811B1