反应 #64258

反应方程式

2-hydroxypropyl carbamate

methacrylic anhydride

→

2-hydroxypropyl carbamate methacrylate

收率 67.2%

溶剂

pyridine

反应条件

后处理

1. 1
   其他A four-necked, five-liter round-bottomed reaction flask equipped with a thermometer, condenser, mechanical stirrer, and air sparger
2. 2
   workup.WAITDuring this heating period
3. 3
   其他during the course of the reaction
4. 4
   其他the reaction mass is sparged with air
5. 5
   其他is held at 65° C. until the concentration of methacrylic anhydride
6. 6
   洗涤The resulting product is then washed with a saturated solution of sodium carbonate
7. 7
   其他the aqueous layer removed from the solids by decantation
8. 8
   洗涤The resulting solid product is then washed twice with a total of two gallons of distilled water
9. 9
   温度by heating the wash water to 50° C
10. 10
    workup.STIRRINGDuring the washing procedure, the melted solids are well stirred
11. 11
    其他to separate from the molten organic material
12. 12
    其他decanted before the desired product
13. 13
    其他The wet product is dried overnight in a hood

实验过程

A four-necked, five-liter round-bottomed reaction flask equipped with a thermometer, condenser, mechanical stirrer, and air sparger is charged with 1,920 g (16.1 moles) of 2-hydroxypropyl carbamate, 2,236 g (14.5 moles) of distilled methacrylic anhydride, 83 g of anhydrous pyridine, and 4.2 g (1,000 parts per million) methoxyhydroquinone. The reaction mass is stirred and slowly heated to 65° C. with a hot-water bath. During this heating period and during the course of the reaction, the reaction mass is sparged with air. The reaction mass is held at 65° C. until the concentration of methacrylic anhydride decreased to less than 1.5 percent by weight. The resulting product is then washed with a saturated solution of sodium carbonate, and the aqueous layer removed from the solids by decantation. This washing procedure is repeated two more times to neutralize all of the methacrylic acid. The resulting solid product is then washed twice with a total of two gallons of distilled water. For each wash, the solids are melted by heating the wash water to 50° C. During the washing procedure, the melted solids are well stirred and the aqueous material is allowed to separate from the molten organic material and decanted before the desired product resolidifies. The wet product is dried overnight in a hood to yield 2,000 g of anhydrous 2-hydroxypropyl carbamate methacrylate that analysis indicates has a 97% purity.

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