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ChemicalBook CAS DataBase List tert-Butyl diethylphosphonoacetate
27784-76-5

tert-Butyl diethylphosphonoacetate synthesis

5synthesis methods
Triethyl phosphite (485 g) is warmed up to 90°C under N2 atmosphere in a three-necked round-bottomed flask, and /-butyl bromoacetate (541 g) is added dropwise into the system within 2 h. Then, the mixture is stirred at 90°C for around 4 hours and cooled to room temperature. The obtained mixture is distilled under vacuo to remove compounds with low boiling points, and the residue is collected as a colorless liquid tert-butyl diethylphosphonoacetate in 97 percent yield (680 g).
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Yield:27784-76-5 97%

Reaction Conditions:

at 90; for 6 h;Inert atmosphere;

Steps:

2 Example 2 Preparation of Compound 2 (R3 = Et)(Diethoxy-phosphoryl)-acetic acid tert-butyl ester
Triethyl phosphite (485 g) is warmed up to 90°C under N2 atmosphere in a three-necked round-bottomed flask, and /-butyl bromoacetate (541 g) is added dropwise into the system within 2 h. Then the mixture is kept stirring at 90°C for around 4 h, and then cooled to room temperature. The obtained mixture is distilled under vacuo to remove compounds with low boiling point, and the residue is collected as a colorless liquid compound 5 in 97% yield (680 g) and >98% GC purity.

References:

BOEHRINGER INGELHEIM INTERNATIONAL TRADING (SHANGHAI) CO., LTD:;BOEHRINGER INGELHEIM INTERNATIONAL GMBH;ZHENG, Juncheng;DENG, Da;LV, Guanghua;YAN, Jun;BRANDENBURG, Joerg;KROEBER, Jutta;SCHOLZ, Ulrich WO2015/101554, 2015, A1 Location in patent:Page/Page column 17

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