반응 #642385

반응 방정식

2,2-adamantane dimethanol

methacrylic acid

toluene

→

target compound

수율 33.4%

(2-hydroxymethyl-2-adamantyl)-methyl methacrylate

수율 33.4%

용매

water

반응 조건

후처리

1. 1
   기타formed
2. 2
   기타was azeotroped off
3. 3
   기타resumed room temperature
4. 4
   여과it was filtered through Celite
5. 5
   농축The filtrate was concentrated in vacuum
6. 6
   workup.ADDITION300 g of hexane was added to the
7. 7
   농축concentrate for recrystallization
8. 8
   기타The crystals were recovered
9. 9
   기타dried in vacuum

실험 절차

A mixture of 100 g of 2,2-adamantane dimethanol, 48.2 g of methacrylic acid, 20 g of toluene, 25 g of acidic ion-exchange resin Amberlist-15, and 0.1 g of 2,2′-methylenebis(6-t-butyl-p-cresol) was heated at 120° C. for 6 hours while the water being formed was azeotroped off. After the reaction mixture resumed room temperature, it was filtered through Celite. The filtrate was concentrated in vacuum. 300 g of hexane was added to the concentrate for recrystallization. The crystals were recovered and dried in vacuum, obtaining 45.0 g (yield 33%) of the target compound. The spectral data of this compound were identical with those of the product in Synthesis Example 1-2.

출처