反应 #742294

反应方程式

N-ethyl-N-isopropylpropan-2-amine

tert-butylchlorodimethylsilane

azetidin-3-ol hydrochloride

→

product

收率 74.0%

Azetidin-3-yloxy-tert-butyl-dimethylsilane

收率 74.0%

溶剂

DCM

DCM

反应条件

后处理

1. 1
   浓缩The reaction mixture was concentrated
2. 2
   workup.ADDITIONdiluted with EtOAc (75 mL)
3. 3
   洗涤washed sequentially with saturated NaHCO3 (25 mL), water (20 mL), and saturated brine (20 mL)
4. 4
   干燥The organic layer was dried (MgSO4)
5. 5
   过滤filtered
6. 6
   其他evaporated

实验过程

A solution of tert-butylchlorodimethylsilane (12.01 g, 79.69 mmol) in DCM (20 mL) was added dropwise to a stiffed solution of azetidin-3-ol hydrochloride (CAS no. 18621-18-6) (8.73 g, 79.69 mmol) and anhydrous N-ethyl-N-isopropylpropan-2-amine (34.1 mL, 199.22 mmol) in DCM (20 mL) cooled to 10° C., over a period of 2 minutes under nitrogen. The resulting solution was stirred at ambient temperature for 20 hours. The reaction mixture was concentrated, diluted with EtOAc (75 mL), and washed sequentially with saturated NaHCO3 (25 mL), water (20 mL), and saturated brine (20 mL). The organic layer was dried (MgSO4), filtered and evaporated to afford the product (11.1 g, 74%). 1H NMR (400 MHz, CDCl3) δ 0.04 (6H, s), 0.87 (9H, m), 2.80 (1H, s), 3.57-3.61 (2H, m), 3.67-3.71 (2H, m), 4.57-4.64 (1H, m).

来源