反应 #657331

反应方程式

4-benzyloxycarbonylamino-piperidine-1-carboxylic acid tert-butyl ester

trifluoroacetic acid

→

brown oil

收率 104.9%

Piperidin-4-yl-carbamic acid benzyl ester

收率 104.9%

溶剂

dichloromethane

反应条件

后处理

1. 1
   浓缩was concentrated
2. 2
   workup.DISSOLUTIONThe residue was dissolved in water (100 mL)
3. 3
   workup.ADDITIONthen basified to pH 11 via addition of solid potassium carbonate
4. 4
   萃取The resulting solution was extracted with dichloromethane (2×150 mL)
5. 5
   干燥they were dried (Na2SO4)
6. 6
   过滤filtered
7. 7
   浓缩concentrated
8. 8
   其他the observed particulates were removed via filtration through a glass frit
9. 9
   浓缩The solution was concentrated

实验过程

To a solution of 4-benzyloxycarbonylamino-piperidine-1-carboxylic acid tert-butyl ester (20.4 g, crude from previous step) in dichloromethane (100 mL) at 23° C. was added trifluoroacetic acid (40 mL). After stirring for 45 min the reaction mixture was concentrated. The residue was dissolved in water (100 mL) then basified to pH 11 via addition of solid potassium carbonate. The resulting solution was extracted with dichloromethane (2×150 mL). The organic extracts were extremely cloudy; they were dried (Na2SO4), filtered and concentrated. The residue was dissolved/suspended in chloroform (70 mL) and the observed particulates were removed via filtration through a glass frit. The solution was concentrated to give 15 g of brown oil. This material was used without purification in the subsequent step.

来源