反应详情

To N-Boc-(2S,4R)-4-hydroxy-2-hydroxymethylpyrrolidine (0.199 g, 0.92 mmol) in DMF (2 ml) was added imidazole (0.125 g) and t-butyldimethylsilyl chloride (0.14 g). After 1.5 h, the reaction was concentrated by evaporation under reduced pressure, and the residue dissolved in diethyl ether, washed with water and brine, dried and evaporated. Purification by chromatography on silica gel eluting with 0-30% ethyl acetate in hexane gave the title material, (0.15 g, 49%). NMR (CDCl3) 0.02 (s, 3H), 0.03 (s, 3H), 0.9 (s, 9H), 1.45 (s, 9H), 1.9 (bm, 9H), 2.2 (bm, 1H), 3.3-4.0 (bm, 5H), 4.5 (m, 1H).

1. concentrationthe reaction was concentrated by evaporation under reduced pressure
2. dissolutionthe residue dissolved in diethyl ether
3. washwashed with water and brine
4. customdried
5. customevaporated
6. customPurification by chromatography on silica gel eluting with 0-30% ethyl acetate in hexane