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ChemicalBook CAS DataBase List [[2-(6-Amino-9H-purin-9-yl)ethoxy]methyl]phosphonic acid diethyl ester

[[2-(6-Amino-9H-purin-9-yl)ethoxy]methyl]phosphonic acid diethyl ester synthesis

6synthesis methods
31618-90-3 Synthesis
Diethyl (tosyloxy)methylphosphonate

31618-90-3
426 suppliers
$5.00/5g

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Yield: 70%

Reaction Conditions:

with magnesium 2-methylpropan-2-olate in N,N-dimethyl-formamide at 80; for 12 h;

Steps:

1.4 Synthesis of 9- [2- (diethylphosphonoylmethoxy) ethyl] adenine
In the 1L the reaction bottle, are respectively added into DMF 182 ml, 9-(2-hydroxyethyl)adenine 45.6g (0.254 µM), tertiary butyl alcohol magnesium 21.4g (0.125 µM), to be slowly heated to 80 °C, paratoluene sulfonyl oxygen methoxy phosphine acid diethyl ester 120.8g (0.375 µM) is slowly added to the reaction solution, the dropwise to continue the reaction 12h, glacial acetic acid in and to the neutral, pressure reducing recovery DMF to dry, adding water 114 ml, dichloromethane continuous extraction 8h, pressure reducing recycling the organic phase solvent, residues adding toluene freezing overnight. Filtering, the filter cake is dried to obtain 58g white powder solid that is the target product, yield 70%.

References:

Chenxin Pharmaceutical Co., Ltd.;Lu Min;Li Zhongjing;Yuan Hongyu;Lu Xiulian;Du Zhenxin CN106699814, 2017, A Location in patent:Paragraph 0022-0023

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