反应 #2487454

反应方程式

t-butyldimethylsilyl trifluoromethanesulfonate

2,6-Lutidine

methylene chloride

benzyl 3-hydroxy-3-methylbutyrate

→

benzyl 3-(t-butyldimethylsilyloxy)-3-methylbutyrate

溶剂

ethyl acetate

反应条件

后处理

1. 1
   其他obtained in the step 1
2. 2
   温度with cooling with ice
3. 3
   workup.STIRRINGstirred for 1hour
4. 4
   温度with cooling on ice
5. 5
   其他The reaction liquid
6. 6
   洗涤washed with water, aqueous saturated ammonium chloride solution and aqueous saturated sodium chloride solution
7. 7
   干燥dried over anhydrous magnesium sulfate
8. 8
   浓缩concentrated
9. 9
   其他4.5g of the residue was purified through silica gel column chromatography

实验过程

2,6-Lutidine (3.6g) was added to an anhydrous methylene chloride solution of benzyl 3-hydroxy-3-methylbutyrate (3.5g) obtained in the step 1, and stirred with cooling with ice. t-butyldimethylsilyl trifluoromethanesulfonate (3.9mL) was gradually added dropwise thereto, and stirred for 1hour with cooling on ice and then for 2hours at room temperature. The reaction liquid was diluted with ethyl acetate, then washed with water, aqueous saturated ammonium chloride solution and aqueous saturated sodium chloride solution, then dried over anhydrous magnesium sulfate and concentrated. 4.5g of the residue was purified through silica gel column chromatography to give benzyl 3-(t-butyldimethylsilyloxy)-3-methylbutyrate (2.62g) as a colorless oil.

来源