反応 #955902

反応方程式

isosorbide

itaconic acid

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product

収率 94.5%

Isosorbide Itaconic Acid

収率 94.5%

反応条件

後処理

1. 1
   その他To a 3-neck 250 mL round-bottomed flask equipped with a dean stark trap and a condenser
2. 2
   温度The temperature was then raised to 180° C.
3. 3
   その他condensation
4. 4
   その他began around 150° C
5. 5
   workup.WAITThereafter, vacuum (1-2 mm-Hg) was applied for ˜30 min
6. 6
   その他A total of 3.0 mL water was collected in the dean stark trap
7. 7
   温度The reaction mixture was cooled under argon to ˜100° C.
8. 8
   温度cooled to room temperature

実験手順

To a 3-neck 250 mL round-bottomed flask equipped with a dean stark trap and a condenser was added isosorbide (40.0 g, 273.9 mmol, obtained from Archer Daniels, Midland, Ill.), itaconic acid (32.39 g, 248.9 mmol, obtained from Sigma-Aldrich), and FASCAT 4201 dibutyl tin oxide catalyst (0.07 g, 0.1 wt %, obtained from Arkema Inc.). The mixture was slowly heated under argon to 120° C., during which time the reagents melted. The temperature was then raised to 180° C., and condensation began around 150° C. The reaction mixture was stirred at 180° C. overnight (˜20 h). Thereafter, vacuum (1-2 mm-Hg) was applied for ˜30 min. A total of 3.0 mL water was collected in the dean stark trap. The reaction mixture was cooled under argon to ˜100° C. and discharged into an aluminum tray and cooled to room temperature to give 65 g of product as a glassy material. Tg(DSC)=19.5° C.; viscosity @130° C.=769 cps; viscosity @70° C.=6.63×105 cps. Mn(GPC)=689; Mw(GPC)=1245; Pd(GPC)=1.80.

出典