反应详情

温度

0 °C

2-(3,5-Dichlorophenoxy)-N-(1-tert-butyldimethylsilyloxy-4-methylpent-2-yn-4-yl)butyramide (prepared as described in Example 1; 3.35 g) in tetrahydrofuran (60 ml) was stirred at 3-5° C. and a solution of tetra n-butylammonium fluoride (14.6 ml of 1M solution in tetrahydrofuran) was added dropwise over 5 minutes. On completion of the addition, the mixture was stirred for 0.5 hour at 0° C., 2 hours at ambient temperature and stored for 18 hours. The solvent was evaporated under reduced pressure and the residue partitioned between ethyl acetate and aqueous ammonium chloride. The organic phase was separated, washed with aqueous ammonium chloride, brine, dried over magnesium sulphate and evaporated under reduced pressure to give a colourless solid that was fractionated by chromatography (silica; hexane/ethyl acetate, 2:1 by volume) to give the required product as a colourless solid (2.01 g) mp 104-106° C.

1. additionOn completion of the addition
2. waitstored for 18 hours
3. customThe solvent was evaporated under reduced pressure
4. customthe residue partitioned between ethyl acetate and aqueous ammonium chloride
5. customThe organic phase was separated
6. washwashed with aqueous ammonium chloride, brine
7. dry with materialdried over magnesium sulphate
8. customevaporated under reduced pressure
9. customto give a colourless solid