反应详情

17.43 g (0.100 mol) of 1,3-bis-(propylamino-propan-2-ol was mixed with 110 ml (0.220 mol) of 2N caustic soda solution and stirred at room temperature for 10 minutes. The mixture was cooled to 0° C. A solution of 19.46 g (0.215 mol) of acrylic acid chloride and 20 mg of BHT in 120 ml of chloroform was added dropwise at 0° C. within 3 hours 30 minutes. After the addition was completed the reaction mixture was stirred at 0° C. for 2 hours 30 minutes. Organic and aqueous phases were separated. The aqueous phase was saturated with NaCl and extracted with 5×80 ml of methylene chloride. The combined organic phases were dried over Na2SO4, filtered, concentrated in a rotary evaporator after addition of 20 mg of BHT and dried in a fine vacuum. The raw product was purified by means of two-fold column chromatography (silica gel 60, 0.035-0.070 mm, ethyl acetate). 11.92 g (42.2 mmol; 42%) of the pure product was obtained as a yellowish oil.

1. temperatureThe mixture was cooled to 0° C
2. additionAfter the addition
3. stirringwas stirred at 0° C. for 2 hours 30 minutes
4. customOrganic and aqueous phases were separated
5. extractionextracted with 5×80 ml of methylene chloride
6. dry with materialThe combined organic phases were dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated in a rotary evaporator
9. additionafter addition of 20 mg of BHT
10. customdried in a fine vacuum
11. customThe raw product was purified by means of two-fold column chromatography (silica gel 60, 0.035-0.070 mm, ethyl acetate)
12. custom11.92 g (42.2 mmol; 42%) of the pure product was obtained as a yellowish oil