Azobisisobutyronitrile → 3-(Bromomethyl)-1-benzothiophene

3-Methylbenzo[b]thiophene (9.9 g, 67 mmol) is heated in carbon tetrachloride (133 ml) to near reflux in the presence of n-bromosuccinimide (11.9 g, 67 mmol, 1.0 eq.). 2,2′Azobisisobutyronitrile (2.2 g, 13.3 mmol, 0.2 eq.) is added and the resulting mixture is refluxed for two hours. After cooling, the reaction mixture is filtered through a glass-fritted funnel, and the filtrate is concentrated. The residue is triturated with petroleum ether and toluene to afford 6.42 g of 3-Bromomethylbenzo[b]thiophene (42%). The title amine is prepared from 3-(bromomethyl)-benzo[B]thiophene in a similar fashion as described in U.S. Pat. No. 4,321,398.

1. temperaturethe resulting mixture is refluxed for two hours
2. temperatureAfter cooling
3. filtrationthe reaction mixture is filtered through a glass-fritted funnel
4. concentrationthe filtrate is concentrated
5. customThe residue is triturated with petroleum ether and toluene

ORDレコード

ord-72b57041208a4f0189159b5c6e89268c

出典データセット

uspto-grants-2005_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06911463B2