Hydrochloric Acid → (4-Bromo-2-chlorophenyl)methanamine

To a solution of 4-bromo-2-chlorobenzonitrile (2 g, 9.24 mmol) in Tetrahydrofuran (THF) (10 ml) was added aluminum hydride (37.0 ml, 18.48 mmol) in THF. The reaction mixture was acidified with 1N HCl to pH=4. The mixture was washed with ether (2×50 ml). The aqueous layer was separated and it was adjusted with 1N NaOH to pH=10. The mixture was extracted with ether. The organic layer was separated and dried over Na2SO4. The solvent was evacuated to give 1-(4-bromo-2-chlorophenyl)methanamine (1.8 g, 8.2 mmol, 88%). MS (ES+): m/e 220, 222 [M+H]+.

1. washThe mixture was washed with ether (2×50 ml)
2. customThe aqueous layer was separated
3. extractionThe mixture was extracted with ether
4. customThe organic layer was separated
5. dry with materialdried over Na2SO4
6. customThe solvent was evacuated

ORDレコード

ord-32a07a1560ec4257ba60fb589ff51fb1

出典データセット

uspto-grants-2012_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08212032B2