反应详情

4-{4-[(7-Methoxy-3-methyl-1H-indole-2-carbonyl)-amino]-phenyl}-piperazine-1-carboxylic acid tert-butyl ester (139 mg, 0.3 mmol) (see example 1) was stirred in 5 mL of 1:3 TFA/CH2Cl2 at r.t. overnight, then concentrated. The residue was dissolved in 5 mL of 30:70 diisopropylethylamine/anhydrous dichloromethane, 2,2-dimethyl-succinic acid (72 mg, 0.49 mmol), N-hydroxybenzotriazole (61 mg, 0.45 mmol) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (86 mg, 0.45 mmol) were added. The reaction mixture was stirred at room temperature overnight. After the reaction, solvent was evaporated. The resulted mixture was mixed with water and extracted with ethyl acetate twice. The organic layers were collected, combined, washed with brine before dried over sodium sulfate, and then concentrated to give a solid. The crude product was purified by reverse phase HPLC (10%-80% acetonitrile in water) to gave 7 mg of 4-(4-{4-[(7-methoxy-3-methyl-1H-indole-2-carbonyl)-amino]-phenyl}-piperazin-1-yl)-2,2-dimethyl-4-oxo-butyric acid. LCMS calcd for C27H32N4O5 (m/e) 492, obsd 493 (M+H).

1. concentrationconcentrated
2. additionwere added
3. customAfter the reaction, solvent
4. customwas evaporated
5. additionThe resulted mixture was mixed with water
6. extractionextracted with ethyl acetate twice
7. customThe organic layers were collected
8. washwashed with brine
9. dry with materialbefore dried over sodium sulfate
10. concentrationconcentrated
11. customto give a solid
12. customThe crude product was purified by reverse phase HPLC (10%-80% acetonitrile in water)