反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
3.87 grams (33.9 mmol, MW: 114.10) 4-vinyl-1,3-dioxaolane-2-one, 5.0 grams (30.8 mol, MW: 162.25) butyl-3-mercaptopropionate and 0.505 grams (3.1 mmol, MW: 164.21) 2,2′-azobis(2-methylpropionitrile) (AIBN) were charged in a 25 milliliter thick sealed glass reactor. After addition, the reaction mixture was stirred for 22 hours at 110° C. The reaction was then stopped and cooled down to room temperature. The excess of unreacted 4-vinyl-1,3-dioxaolane-2-one was removed by air bath oven at 180° C. under vacuum for 1 hour. The final product was determined by IR, 13CNMR. Yield: 4.26 grams (50%). IR: (cm−1) 2960, 2933, 2873, 1803, 1731, 1456, 1390, 1351, 1246, 1169, 1065, 772. 13C NMR (CDCl3): 171.7, 154.7, 124.6, 113.4, 75.4, 69.2, 64.5, 35.0, 33.9, 30.5, 27.2, 19.1, 13.7.
WORKUP
后处理
- customthick sealed glass reactor
- additionAfter addition
- temperaturecooled down to room temperature
- customThe excess of unreacted 4-vinyl-1,3-dioxaolane-2-one was removed by air bath oven at 180° C. under vacuum for 1 hour