3,3'-[[2,2-bis[(allyloxy)methyl]-1,3-propanediyl]bis(oxy)]dipropene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The procedure used was identical to that set forth in Example 4, except that 107 g of hexadecyl mercaptan (0.417 moles) was reacted with 29.64 g of pure pentaerythritol tetraallyl ether (0.1 moles). The crude product was recrystallized three times in 300 ml of hexane yielding 57 g of white solid having a melting point 55°-57° C. The elemental analysis found: C-73.4%, H-11.9%, S-10.0%, calculated for C88H164S4 (theoretical C-73.12%, H-12.4%, S-9.64% and O-4.81%). The crude product was recrystallized three times in 300 ml of hexane yielding 57 g of white solid

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The procedure used was identical to that set forth in Example 4, except that 107 g of hexadecyl mercaptan (0.417 moles) was reacted with 29.64 g of pure pentaerythritol tetraallyl ether (0.1 moles). The crude product was recrystallized three times in 300 ml of hexane yielding 57 g of white solid having a melting point 55°-57° C. The elemental analysis found: C-73.4%, H-11.9%, S-10.0%, calculated for C88H164S4 (theoretical C-73.12%, H-12.4%, S-9.64% and O-4.81%). The crude product was recrystallized three times in 300 ml of hexane yielding 57 g of white solid

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 30.7 g (0.12 mol) of pentaerythritol triallylether was dissolved in 100 ml of dry THF and 4.4 g (0.18 mol) of NaH was added in small portions while stirring. After gas evolution had ceased, 16 ml (0.18 mol) of allyl bromide was added and the reaction mixture was stirred overnight at room temperature. In order to drive the reaction to completion, it was subsequently brought to reflux and stirred for 1 hr. The precipitated salts were removed by filtration over ca. 1 cm of Celite 545 and the solvent and excess allyl bromide were evaporated, yielding 35.3 g (99.5%) of a pale yellow oil. The raw product was dissolved in 100 ml of diethyl ether and washed subsequently with 50 ml of 0.1 M aqueous KHSO4 and 50 ml of saturated aqueous NaHCO3 solution. Drying the organic layer with MgSO4 and evaporation of the solvent yielded 34.4 g (97%) of the pure product. the reaction mixture was stirred overnight at room temperature the reaction to completion, it to reflux stirred for 1 hr The precipitated salts were removed by filtration over ca. 1 cm of Celite 545 the solvent and excess allyl bromide were evaporated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 30.7 g (0.12 mol) of pentaerythritol triallylether was dissolved in 100 ml of dry THF and 4.4 g (0.18 mol) of NaH was added in small portions while stirring. After gas evolution had ceased, 16 ml (0.18 mol) of allyl bromide was added and the reaction mixture was stirred overnight at room temperature. In order to drive the reaction to completion, it was subsequently brought to reflux and stirred for 1 hr. The precipitated salts were removed by filtration over ca. 1 cm of Celite 545 and the solvent and excess allyl bromide were evaporated, yielding 35.3 g (99.5%) of a pale yellow oil. The raw product was dissolved in 100 ml of diethyl ether and washed subsequently with 50 ml of 0.1 M aqueous KHSO4 and 50 ml of saturated aqueous NaHCO3 solution. Drying the organic layer with MgSO4 and evaporation of the solvent yielded 34.4 g (97%) of the pure product. the reaction mixture was stirred overnight at room temperature the reaction to completion, it to reflux stirred for 1 hr The precipitated salts were removed by filtration over ca. 1 cm of Celite 545 the solvent and excess allyl bromide were evaporated

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 250 ml three-necked flask equipped with a magnetic stirrer, a condenser and a nitrogen inlet tube was first purged with nitrogen 107 grams of n-hexadecyl mercaptan (0.417 mole) was then charged and heated to 80° C. To the heated and stirred n-hexadecyl mercaptan, a solution of 0.2 gram of 2,2'-azobis(isobutyronitrile) in 29.64 grams (0.1 mole) of pure pentaerythritol tetraallyl ether was added dropwise over a 15-minute period. One-half hour after this addition was completed, 0.1 gram of 2,2'-azobis(isobutyronitrile) was added. Two more 0.1 gram additions of 2,2'-azobis-(isobutyronitrile) were made at half-hour intervals. After the last addition, the reaction was held at 80° C. for an additional hour. The crude product was recrystallized three times in 300 ml. of hexane yielding 57 grams of a white solid having a melting point of 55°-57° C. The elemental analysis found: C - 73.4%, H - 11.9%, S(total) - 10.0%, and S(mercapto) - 3 ppm. Calculated for C98H164S2 ; C - 73.12%, H-12.43%, S(total) - 9.64% and S(mercapto) - 4 ppm. A 250 ml three-necked flask equipped with a magnetic stirrer, a condenser and a nitrogen inlet tube was then charged To the heated One-half hour after this addition After the last addition the reaction was held at 80° C. for an additional hour The crude product was recrystallized three times in 300 ml

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The procedure used was identical to that set forth in Example 4, except that 107 g of hexadecyl mercaptan (0.417 moles) was reacted with 29.64 g of pure pentaerythritol tetraallyl ether (0.1 moles). The crude product was recrystallized three times in 300 ml of hexane yielding 57 g of white solid having a melting point 55°-57° C. The elemental analysis found: C-73.4%, H-11.9%, S-10.0%, calculated for C88H164S4 (theoretical C-73.12%, H-12.4%, S-9.64% and O-4.81%). The crude product was recrystallized three times in 300 ml of hexane yielding 57 g of white solid