Water → 4-Bromo-2-(methylsulfonamido)benzoic acid

Methyl 2-amino-4-bromobenzoate (1 g) was dissolved in tetrahydrofuran (15 mL), triethylamine (4.2 mL) and methanesulfonyl chloride (0.74 mL) were added, and the mixture was stirred at room temperature for 6 hr. Water was added to the reaction mixture, and the mixture was extracted with chloroform. After evaporation of the solvent, to the residue were added methanol (20 mL) and 1N aqueous sodium hydroxide solution (13 mL), and the mixture was stirred at 50-60° C. After neutralizing with 1N hydrochloric acid, the precipitated solid was collected by filtration to give the title compound (964 mg).

1. extractionthe mixture was extracted with chloroform
2. customAfter evaporation of the solvent
3. additionto the residue were added methanol (20 mL) and 1N aqueous sodium hydroxide solution (13 mL)
4. stirringthe mixture was stirred at 50-60° C
5. filtrationthe precipitated solid was collected by filtration

ORD-Eintrag

ord-9508b847c23b401ea2a18cf38e45e780

Quelldatensatz

uspto-grants-2014_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08816079B2