Water → HCID 54752976, Verbindung

Temperatur

30 °C

DBU (211 ml) was added to a solution of (3-bromophenyl) (4-chloro-2-hydroxy-5-methylphenyl)methanone (170 g) in acetonitrile (510 ml) at 25 to 30° C. Then, a solution of ethyl succinic chloride (146 g) in acetonitrile (340 ml) was added dropwise over 30 minutes at 25 to 40° C. After the drop was completed, the mixture was stirred at 30° C. for 1 hour. Water (94 ml) was added dropwise keeping the reaction solution at 25 to 30° C. After the mixture was stirred at the same temperature for 1 hour, the resulting crystals were filtered, and washed with a mixture of acetonitrile and water (9/1, 170 ml) four times, dried under reduced pressure to obtain the title compound (174 g, yield 76.7%).

1. customat 25 to 30° C
2. stirringAfter the mixture was stirred at the same temperature for 1 hour
3. filtrationthe resulting crystals were filtered
4. washwashed with a mixture of acetonitrile and water (9/1, 170 ml) four times
5. customdried under reduced pressure

ORD-Eintrag

ord-3e8f19f522cd4c56b4b8ec5deeab5cb2

Quelldatensatz

uspto-grants-2009_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07541478B2