Methanol → 3-Bromo-4-methoxyaniline

2-Bromo-1-methoxy-4-nitrobenzene (2.50 g, 10.8 mmol), SnCl2.2H2O (12.2 g, 53.9 mmol), and MeOH (30 mL) were combined and allowed to stir for 3 h at ambient temperature. To the mixture was added H2O (100 mL) and EtOAc (100 mL) resulting in the formation of a thick emulsion. To this was added sat. aq. NaHCO3 (30 mL). The layers were separated and the aqueous layer was extracted with EtOAc (3×30 mL). The organics were combined and dried over MgSO4 before being filtered. Concentration of the filtrate in vacuo gave 2.02 g of an off-white solid. This material was used without further purification.

1. customresulting in the formation of a thick emulsion
2. customThe layers were separated
3. extractionthe aqueous layer was extracted with EtOAc (3×30 mL)
4. dry with materialdried over MgSO4
5. filtrationbefore being filtered

ORDレコード

ord-a48eb89408e442eaa73e43e78766a091

出典データセット

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08846753B2