Methacryloyl chloride → 2-Ethyl-2-methacryloyloxyadamantane

HRID 1699595

反応式

HRID 1699595 の反応式
[CH:1]12[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[C:2]1=[O:11])[CH2:8]2.[CH2:12]([Li])[CH3:13].[C:15](Cl)(=[O:19])[C:16]([CH3:18])=[CH2:17]>C(OCC)C>[C:15]([O:11][C:2]1([CH2:12][CH3:13])[CH:3]2[CH2:9][CH:7]3[CH2:6][CH:5]([CH2:10][CH:1]1[CH2:8]3)[CH2:4]2)(=[O:19])[C:16]([CH3:18])=[CH2:17]

参加物

5

反応物 3

HCID 13528Methacryloyl chlorideHCID 64151AdamantanoneHCID 178506846HCID 178506846、化合物

生成物 1

HCID 98136452-Ethyl-2-methacryloyloxyadamantane

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
0 °C

実験手順

A solution was prepared by adding 50 parts of diethyl ether to 31.1 parts of 2-adamantanone. While keeping the temperature of the solution at or under 10° C., 200 ml of a diethyl ether solution containing ethyl lithium at a concentration of 1.14 mole/liter was added dropwise thereto. The solution was stirred at 0° C. for 2 hours, and then, while keeping the temperature of the solution at or under 10° C., 26.2 parts of methacryloyl chloride (1.2 mole based on 2-methyl-2-adamantanol) was added dropwise. After the completion of addition, the solution was stirred at room temperature for 12 hours. Then precipitated inorganic salts were removed by filtration. The organic layer was washed with 5% aqueous sodium hydrogen carbonate solution and then washed twice with water. The organic layer was concentrated and distilled under reduced pressure to give 2-ethyl-2-adamantyl methacrylate represented by the following formula:

後処理

  1. customA solution was prepared
  2. customunder 10° C.
  3. additionwas added dropwise
  4. customunder 10° C.
  5. additionAfter the completion of addition
  6. stirringthe solution was stirred at room temperature for 12 hours
  7. customThen precipitated inorganic salts
  8. customwere removed by filtration
  9. washThe organic layer was washed with 5% aqueous sodium hydrogen carbonate solution
  10. washwashed twice with water
  11. concentrationThe organic layer was concentrated
  12. distillationdistilled under reduced pressure

出典と根拠

ORDレコード
ord-615dc07fbf1a43a4b60b86f8dee65035
出典データセット
uspto-grants-2002_02
特許番号
US06348297B1

関連ノート

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