反应 #1244252

ord-bc1182f303b44d2eb06e98753e7b1824

反应方程式

CCN(CC)CC
triethyl amine
OCCOCCOCCOCCO
Tetraethylene glycol
CC(C)(C)[Si](C)(C)Cl
TBDMSCl
CC(C)(C)[Si](C)(C)OCCOCCOCCOCCO
5c
收率 42.0%
CC(C)(C)[Si](C)(C)OCCOCCOCCOCCO
2-(2-{2-[2-(tert-Butyl-dimethyl-silanyloxy)-ethoxy]-ethoxy}-ethoxy)-ethanol
收率 42.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他After standard workup with dichloromethane, the residue was purified by silica gel column chromatography (50% ethyl acetate in hexane)

实验过程

Tetraethylene glycol, 4c (1.12 g, 5.77 mmol) and TBDMSCl (0.87 g, 5.77 mmol) were dissolved in dichloromethane (25 ml) followed by triethyl amine (1.46 g, 14.4 mmol). The solution was stirred at room temperature for 2 hours. After standard workup with dichloromethane, the residue was purified by silica gel column chromatography (50% ethyl acetate in hexane) to afford 5c (744 mg, 42%): 1H NMR δ 3.66 (m, 16H), 2.51 (t, 1H, J=5.86 Hz), 0.89 (s, 9H), 0.07 (s, 6H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07807135B2uspto-grants-2010_10