Trifluoroacetic acid → 3-Bromo-N-methylaniline

3.6 g (12.7 mmol) of tert-butyl (3-bromophenyl)-N-methylcarbamate, prepared in a manner analogous to Example 1b), are dissolved in 15 ml of dichloromethane. 5 ml of trifluoroacetic acid are added and the reaction mixture is stirred at ambient temperature for 1 hour. The reaction is halted by the addition of 50 ml of a saturated sodium hydrogencarbonate solution and then extraction is carried out with ethyl acetate. The organic phases are combined and dried over sodium sulfate. The solvents are evaporated and then the residue is chromatographed on silica gel (heptane/ethyl acetate 50/50). 2.14 g of 3-bromo-N-methylaniline are obtained in the form of an oil. Yield=90%.

1. extractionextraction
2. dry with materialdried over sodium sulfate
3. customThe solvents are evaporated
4. customthe residue is chromatographed on silica gel (heptane/ethyl acetate 50/50)

ORDレコード

ord-c24b085d45fe4a24b8a82edbe47772a9

出典データセット

uspto-grants-2009_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07626054B2