反应详情

To a solution of N-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-terephthalamic acid methyl ester 7 (0.20 g, 0.55 mmol) in MeOH (2 mL) was added an hydroxylamine solution (1.76 M, 2 mL) in MeOH and the reaction mixture was stirred 1 h at room temperature under magnetic stirring. The reaction mixture was adjusted to pH=5, concentrated and the residue was partitioned between EtOAc and H2O. The organic layer was dried with Na2SO4 and the product was crystallized by dissolving the mixture at 80° C. in CH3CN to give N-(1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalen-6-yl)-N′-hydroxyterephthalamide EHT 7706 (0.05 g, 25% yield) as a white solid.

1. concentrationconcentrated
2. customthe residue was partitioned between EtOAc and H2O
3. dry with materialThe organic layer was dried with Na2SO4
4. customthe product was crystallized
5. dissolutionby dissolving the mixture at 80° C. in CH3CN