双(2,4-二叔丁基苯基)季戊四醇二亚磷酸酯reaxys_anonymous_20130827_233434_034[1]

OH
O
HO OH OHO P Oຫໍສະໝຸດ OOP OHO
Rx-ID: 35732637 View in Reaxys 2/2 Yield 22 % Conditions & References Stage 1: With triethylamine, phosphorus trichoride in toluene, Time= 1h, T= 5 °C Stage 2: in toluene, Time= 5h, Reflux Rani, Manju; Shukla, Davender Kumar; Khan, Arif Ali; Asian Journal of Chemistry; vol. 25; nb. 8; (2013); p. 4556 4558,3 View in Reaxys
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2013-08-27 23:34:45
Query
Query Results Date
O
O P O
1. Query
O
P O O
2 reactions in Reaxys
2013-08-27 23h:34m:24s (EST)
Search as: Product, As drawn, No salts, No mixtures
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Copyright © 2013 Reed Elsevier Properties SA. All rights reserved. Authorized use only. Reaxys® and the Reaxys® trademark are owned and protected by Reed Elsevier Properties SA and used under license.
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2013-08-27 23:34:45
OH
Cl
HO OH OH
Cl P Cl
O P
O O
O P O O
HO
Rx-ID: 25040097 View in Reaxys 1/2 Yield Conditions & References Example Name 2 Example Title EXAMPLE 2 EXAMPLE 2 40.8 g (0.3 mol) of pentaerythritol, 123.8 g (0.6 mol) of 2,4-di-tert-butylphenol and 3 g (0.014 mol) of tetraethylammonium bromide in 45 ml of xylene are suspended in a 500 ml reaction flask equipped with an HCl absorber. At 15° to 25° C., 82.3 g (0.6 mol) of phosphorous trichloride are added uniformly over one hour. The temperature is then raised uniformly over two hours to 70° C. Subsequently, a pressure of 120 mbar is applied. Pressure and temperature are maintained for two hours. 200 ml of xylene are then added to dissolve the product of 80° C. The solution is filtered in a distillation flask and the filter residue is washed with 2*50 ml of xylene. At 80° C. and 120 mbar, about 300 ml of xylene are distilled off until the limit of stirrability is reached. Then 400 ml of isopropanol are added rapidly and the suspension is stirred under reflux for 15 minutes at 80° C., then cooled to 20° to 25° C. The product is filtered and washed with 2*70 ml of isopropanol. The filter cake is dried in vacuo at 70° C., affording 133.3 g of 3,9-bis(2,4-di-tert-butylphenoxy)2,4,8,10-tetraoxa-3,9diphosphaspiro[5.5]undecane with a melting point of 174° to 177° C. With tetraethylammonium bromide in hydrogenchloride, anhydrous xylene, isopropyl alcohol Patent; Ciba-Geigy Corporation; US4692540; (1987); (A1) English View in Reaxys