反应详情

温度

50 °C

Concentrated H2SO4 (0.2 ml) was added to a solution of Cbz-Asn-OH (10 g, 37.6 mmol), trityl alcohol (20 g, 75.2 mmol), and acetic anhydride (7.1 ml, 75.2 mmol) in acetic acid (114 ml) and the reaction was stirred for 1 hour at 50° C. The solution was cooled and slowly added to 1.0 L of cold H2O. The white precipitate was filtered, dissolved in EthOAc (250 ml), washed with H2O, dried over Na2SO4 and filtered. The resulting white solid was crystallized from EthOAc/hexane to give 13 g (68%) of a white solid.

1. temperatureThe solution was cooled
2. filtrationThe white precipitate was filtered
3. dissolutiondissolved in EthOAc (250 ml)
4. washwashed with H2O
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customThe resulting white solid was crystallized from EthOAc/hexane