反应详情

To a solution of S-3-(benzyloxycarbonylamino)-3-methylbutyl ethanethioate (45.0 g, 152 mmol, prepared as described in WO 2008/083347) in methanol (300 ml) was added 5.0 M NaOH in H2O (60.0 ml, 300. mmol). The solution was stirred for 1 hour, concentrated in vacuo, diluted with saturated NaHSO4 (200 ml), filtered through a coarse glass funnel, and extracted with 5×100 ml ethyl acetate. The organic layers were combined, washed with 100 ml saturated NaCl, dried on MgSO4, and concentrated in vacuo. The residue was used without further purification (24.10 g, 95.1 mmol, 63%).

1. concentrationconcentrated in vacuo
2. additiondiluted with saturated NaHSO4 (200 ml)
3. filtrationfiltered through a coarse glass funnel
4. extractionextracted with 5×100 ml ethyl acetate
5. washwashed with 100 ml saturated NaCl
6. customdried on MgSO4
7. concentrationconcentrated in vacuo
8. customThe residue was used without further purification (24.10 g, 95.1 mmol, 63%)