反应详情

To a solution of 3.19 g (30.6 mmol) 2,N-dihydroxy-propionamidine in 25 ml pyridine was added 4.3 ml (33.7 mmol) 3-chloro-benzoyl chloride at 0° C. Cooling was removed and the mixture was stirred at room temperature for 25 min and at reflux for 25 min. After cooling the mixture was poured into water and extracted twice with CH2Cl2. The organic phase was dried and concentrated. Recrystallization from heptane/EtOAc afforded 4.12 g (60%) of a white solid. 1H NMR (CDCl3), d (ppm): 1.68 (d, 3 H) 2.67 (m, 1 H) 5.09 (m, 1 H) 7.46 (t, 1 H) 7.56 (d, 1 H) 8.01 (d, 1 H) 8.13 (s, 1 H).

1. temperatureCooling
2. customwas removed
3. temperatureat reflux for 25 min
4. temperatureAfter cooling the mixture
5. additionwas poured into water
6. extractionextracted twice with CH2Cl2
7. customThe organic phase was dried
8. concentrationconcentrated
9. customRecrystallization from heptane/EtOAc