反应 #674318

反应方程式

sodium hydride

DMF

alcohol

(R)—N-Boc-2-hydroxypiperidine

DMF

iodomethane

→

(R)—N-Boc-2-methoxymethylpiperidine

收率 85.0%

反应条件

后处理

1. 1
   温度was cooled with ice
2. 2
   workup.ADDITIONwas added
3. 3
   其他The mixture was quenched with saturated NH4Cl-solution
4. 4
   萃取extracted with EtOAc
5. 5
   洗涤The combined organic extracts were washed with brine
6. 6
   干燥dried over MgSO4
7. 7
   浓缩concentrated under reduced pressure

实验过程

A suspension of sodium hydride (0.13 g, 5.4 mmol) in DMF (4 mL) was cooled with ice and a solution of the intermediate alcohol of Step 2 (0.97 g, 4.5 mmol) in DMF (1 mL) was added dropwise. After stirring for 30 min at room temperature iodomethane (0.96 g, 6.8 mmol) was added and the mixture was stirred over night. The mixture was quenched with saturated NH4Cl-solution and extracted with EtOAc. The combined organic extracts were washed with brine, dried over MgSO4 and concentrated under reduced pressure to leave the crude (R)—N-Boc-2-methoxymethylpiperidine (0.88 g, 85%).

来源