反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Methyl 4-aminocarbonyl-5-(isopropylamino)-2-methylbenzoate (202 mg, 0.81 mmol) was dissolved in methanol (3 mL) and was treated with 1M sodium hydroxide (3 mL, 3 mmol) at 45° C. for 1.5 h. The reaction mixture was cooled to ambient temperature and was concentrated to afford an aqueous residue that was acidified with 1N hydrochloric acid to pH 3. The precipitate was collected by filtration, washed with water and dried to afford 4-aminocarbonyl-5-(isopropylamino)-2-methylbenzoic acid (99.5 mg, 0.42 mmol, 52% yield). 1H NMR (400 MHz, d6-DMSO): δ 12.95 (br s, 1H), 7.90 (br s, 1H), 7.72 (d, 1H), 7.49 (s, 1H), 7.28 (br s, 1H), 7.06 (s, 1H), 3.64-3.54 (m, 1H), 2.33 (s, 3H), 1.15 (s, 3H), 1.14 (s, 3H); MS (EI) for C12H16N2O3: 237 (MH+).
WORKUP
后处理
- concentrationwas concentrated
- customto afford an aqueous residue that
- filtrationThe precipitate was collected by filtration
- washwashed with water
- customdried