反应详情

温度

80 °C

(2R,3R,4R)-3,4-Dibenzyloxy-2-benzyloxymethylpyrrolidine (Compound 1) (1.025 g, 2.5 mmol) was dissolved in methylisobutylketone (15 ml). Triethylamine (0.53 ml, 3.8 mmol) and potassium iodide (0.04 g) were added. The mixture was stirred under a nitrogen atmosphere for 4 hours at 80° C. and 24 hours at room temperature and evaporated in vacuo. Water (40 ml) was added and extraction with methylene chloride (3×40 ml), drying of the organic phases with magnesium sulphate and evaporation of the solvent in vacuo afforded a yellow oil. Purification of the crude product on a silica gel column (Eluent: Heptane/ethyl acetate (9: 1)) gave (2R,3R,4R)-1-allyl-3,4-dibenzyloxy-2-benzyloxymethylpyrrolidine (0.91g, yield: 81%) as an oil.

1. customevaporated in vacuo
2. additionWater (40 ml) was added
3. extractionextraction with methylene chloride (3×40 ml)
4. dry with materialdrying of the organic phases with magnesium sulphate and evaporation of the solvent in vacuo
5. customafforded a yellow oil
6. customPurification of the crude product on a silica gel column (Eluent: Heptane/ethyl acetate (9: 1))