반응 #93596

반응 방정식

methyl angelate

dioctyltin acetate

3-methyl-2-pentenol

→

3-Methyl-2-Pentenyl Angelate

용매

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONA mixture of 22.8 g
2. 2
   기타glass flask, which was equipped with a Soxhlet extractor
3. 3
   온도The above mixture was heated
4. 4
   온도under continuous reflux
5. 5
   기타The mixture resulted from the heating for a total of 17 hours
6. 6
   workup.DISTILLATIONwas subjected to single distillation
7. 7
   기타to give 14.2 g
8. 8
   기타to give 9.70 g
9. 9
   기타Refractive index (D ray, 20° C.)

실험 절차

A mixture of 22.8 g. of methyl angelate, 10 g. of 3-methyl-2-pentenol, 80 ml. of toluene and 1 g. of dioctyltin acetate was placed in a 300 ml. glass flask, which was equipped with a Soxhlet extractor filled on the top with molecular sieve 4A and a reflux cooler. The above mixture was heated under continuous reflux while returning the refluxed liquid through the molecular sieve 4A to the flask. The mixture resulted from the heating for a total of 17 hours was subjected to single distillation to give 14.2 g. of a distillate boiling at 115° C. (22 mmHg). The distillate was further subjected to rectification to give 9.70 g. of a distillate boiling at 115° C. (22 mmHg). Analysis of the compound by gaschromatography (Column: Silicone SE-52, 2%/chromosorb GHP) indicated a purity of 99.403% in terms of the area ratio. Refractive index (D ray, 20° C.) was 1.463. Infrared spectrum (liquid film) had absorptions at 2850-3020, 1720, 1670, 1650, 1455, 1385, 1350, 1255, 1225, 1155, 1080, 1040, 960, 845 and 760 cm-1.

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