ChemicalBook CAS DataBase List Methyldiethoxyphosphine

Methyldiethoxyphosphine synthesis

6synthesis methods

Product Name:Methyldiethoxyphosphine
CAS Number:15715-41-0
Molecular formula:C5H13O2P
Molecular Weight:136.13

589-57-1 Synthesis

589-57-1
169 suppliers
$37.29/5g

676-58-4 Synthesis

676-58-4
287 suppliers
$15.00/25ml

15715-41-0
142 suppliers
$80.90/1g

Yield:15715-41-0 89.3%

Reaction Conditions:

Stage #1:diethyl phosphorylchloridite;methylmagnesium chloride in tetrahydrofuran at -10 - 0; for 2 h;Inert atmosphere;
Stage #2: with dibutyl ether;benzylamine in tetrahydrofuran at -5; for 10 h;Reagent/catalyst;Temperature;

Steps:

1; 3-4; 7-9; 12-19 Preparation of diethyl methyl phosphonite reaction solution:
Under the protection of nitrogen, Add 40mL of tetrahydrofuran and 15.6g (0.1mol) of diethyl phosphonite chloride into a four-necked flask, Cool down to -10°C, 41.1g (0.11mol) of tetrahydrofuran solution containing 20wt% methylmagnesium chloride was added dropwise, Keep temperature -100 and react for 2h, The content of diethyl chlorophosphinate detected by gas chromatography is less than 0.3%, After the reaction is over, a reaction solution of diethyl methylphosphonite is obtained. Add 28 g of butyl ether to the reaction solution of diethyl methyl phosphonite obtained in Example 1, Add 5.4g of benzylamine, keep the temperature at -5°C and stir slowly for 10h, After filtering and drying, anhydrous magnesium chloride with a content of more than 97% is obtained. The filtrate was rectified under reduced pressure, and the 60-70/50mmHg fraction was collected and collected. 12.4 g of diethyl methyl phosphonite was obtained, the gas content was 98.0%, and the yield was 89.3%. According to Kjeldahl nitrogen determination method, the nitrogen content in anhydrous magnesium chloride is 0.18%.

References:

Hebei Weiyuan Biochemical Co., Ltd.;Shi Xiuxiao;Gao Yongmin;Fan Lipan;Li Zhifeng;Li Lihua;Fan Chaohui;Jia Chengguo CN112028936, 2020, A Location in patent:Paragraph 0041-0043; 0047-0052; 0059-0067; 0074-0083

FullText

64-17-5 Synthesis