Sodium Hydroxide → 2-Bromo-4,5,6,7-tetrahydro-1-benzothiophen-4-one

Temperatur

0 °C

6,7-Dihydro-4-Benzo[B]thiophenone (1.5 g, 9.86 mmol) was dissolved in acetic acid (10 mL) and water (10 mL). The mixture was cooled to 0° C. and bromine (0.51 mL, 9.86 mmol) was added drop-wise. After 20 min at 0° C. the reaction was warmed to room temperature and stirred for 18 hr. The reaction mixture was cooled in ice and then treated with 1 M aqueous sodium hydroxide solution until the mixture was basic. A precipitate formed which was collected by filtration, washed with water and dried in a vacuum oven at 50° C. to afford the title compound as a grey solid (2.1 g, 96%).

1. temperatureAfter 20 min at 0° C. the reaction was warmed to room temperature
2. temperatureThe reaction mixture was cooled in ice
3. customA precipitate formed which
4. filtrationwas collected by filtration
5. washwashed with water
6. customdried in a vacuum oven at 50° C.

ORD-Eintrag

ord-5baf4a49a1984e8ea1c043f53543fafe

Quelldatensatz

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09233982B2