反应详情

To a stirred solution of Boc-D-Valine amide (10 g, 46 mMol) in CH2Cl2 (200 mL) was added Triethyloxoniuim hexafluorophosphate (13.0 g, 48 mMol). (The reaction started out as a suspension which gradually cleared.) The reaction was stirred for 48 h at RT, poured into a separatory funnel, washed with 1 N Na2CO3, dried (Na2SO4), filtered and concentrated under vacuum. To the remaining oil was added Benzylamine (5.0 mL, 23 mMol) and EtOH (20 mL). The reaction was stirred at 60° C. for 24 h. After cooling to RT the reaction was evaporated under vacuum. The title compound (14.16 g, >95% pure by LCMS) was obtained without purification as a pale yellow oil which eventually solidified to a waxy solid: MS (ES) m/e 306.4 (M+H)+.

1. additionpoured into a separatory funnel
2. washwashed with 1 N Na2CO3
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated under vacuum
6. stirringThe reaction was stirred at 60° C. for 24 h
7. temperatureAfter cooling to RT the reaction
8. customwas evaporated under vacuum