反应详情

温度

80 °C

DBU (23.5 mL) was added slowly to a solution of cyano-acetic acid tert-butyl ester (8.84 g) in DMF (100 mL) at rt, followed by addition of 1,3-dibromopropane (13.9 g); then the reaction mixture was stirred in an oil bath (bath temperature=80° C.) overnight. The reaction was cooled, diluted with EtOAc, then washed with cold water, dil. NaCl solution; EtOAc phase was dried over anhydrous sodium sulfate, filtered, concentrated, the residue was column purified to give title compound (6.58 g). 1H NMR in CDCl3, δ in ppm: 2.8-2.5 (m, 4H), 2.4-2.2 (m, 2H), 1.51 (s, 9H).

1. temperatureThe reaction was cooled
2. washwashed with cold water, dil. NaCl solution
3. dry with materialEtOAc phase was dried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. custompurified