반응 #742294

반응 방정식

N-ethyl-N-isopropylpropan-2-amine

tert-butylchlorodimethylsilane

azetidin-3-ol hydrochloride

→

product

수율 74.0%

Azetidin-3-yloxy-tert-butyl-dimethylsilane

수율 74.0%

용매

DCM

DCM

반응 조건

후처리

1. 1
   농축The reaction mixture was concentrated
2. 2
   workup.ADDITIONdiluted with EtOAc (75 mL)
3. 3
   세척washed sequentially with saturated NaHCO3 (25 mL), water (20 mL), and saturated brine (20 mL)
4. 4
   건조The organic layer was dried (MgSO4)
5. 5
   여과filtered
6. 6
   기타evaporated

실험 절차

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).

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