反应详情

A stirred solution of 3,3-dicyclohexylpropionyl chloride (6.1 g, 0.063 mol) in 70 ml of chloroform was treated portionwise at 7°-12° C. with a solution of 8.3 g (0.063 mol) of glycine tert-butyl ester and 8.9 ml (0.064 mol) of triethylamine in 30 ml of chloroform. After the addition, the solution was stirred at room temperature for 2 hours, kept overnight, refluxed for 0.5 hours, cooled, washed with water (5×25 ml), dried (magnesium sulfate), and the solvent removed on a rotary evaporator, to give a light yellow viscous oil. The latter, which crystallized partly on standing, was dissolved in 50 ml of boiling hexane, cooled, seeded, and rubbed; a crystalline solid gradually separated. After crystallizing at room temperature and cooling overnight, the voluminous colorless solid was filtered, washed with cold hexane and air-dried (13.3 g, melting point 72°-74° C. s, 69° C.).

1. additionAfter the addition
2. waitkept overnight
3. temperaturerefluxed for 0.5 hours
4. temperaturecooled
5. washwashed with water (5×25 ml)
6. dry with materialdried (magnesium sulfate)
7. customthe solvent removed on a rotary evaporator
8. customto give a light yellow viscous oil
9. customThe latter, which crystallized partly
10. dissolutionwas dissolved in 50 ml of boiling hexane
11. temperaturecooled
12. customa crystalline solid gradually separated
13. customAfter crystallizing at room temperature
14. temperaturecooling overnight
15. filtrationthe voluminous colorless solid was filtered
16. washwashed with cold hexane
17. customair-dried (13.3 g, melting point 72°-74° C. s, 69° C.)