反应详情

2 g of (N-Boc)-4-cyanophenylalanine, 2.32 g of TBTU, 2.40 ml of DIPEA and 806 mg of N,O-dimethylhydroxylamine hydrochloride are mixed together in 30 ml of DCM. After stirring for 24 hours at RT, the reaction mixture is concentrated to dryness and the residue is then extracted with EtOAc. The organic phase is washed with a pH 2 buffer solution, a saturated NaHCO3 solution and then a saturated NaCl solution. The expected compound crystallizes from a mixture of isopropyl ether and pentane (1.89 g).

1. concentrationthe reaction mixture is concentrated to dryness
2. extractionthe residue is then extracted with EtOAc
3. washThe organic phase is washed with a pH 2 buffer solution
4. customThe expected compound crystallizes from a mixture of isopropyl ether and pentane (1.89 g)