Triethylamine → 2-Methyl-2-adamantyl methacrylate

HRID 1265960

반응식

HRID 1265960 반응식
[CH3:1][C:2]1([OH:12])[CH:9]2[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:11][CH:3]1[CH2:4]3)[CH2:8]2.C(N(CC)CC)C.[C:20](Cl)(=[O:24])[C:21]([CH3:23])=[CH2:22]>C(C(C)=O)C(C)C>[C:20]([O:12][C:2]1([CH3:1])[CH:3]2[CH2:11][CH:7]3[CH2:6][CH:5]([CH2:10][CH:9]1[CH2:8]3)[CH2:4]2)(=[O:24])[C:21]([CH3:23])=[CH2:22]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 1365452-Methyl-2-adamantanol

생성물 1

HCID 98375662-Methyl-2-adamantyl methacrylate수율 75%

시약·촉매·용매 1

HCID 7909Methyl Isobutyl Ketone용매

실험 절차

Into a reaction vessel were charged 83.1 parts of 2-methyl-2-adamantanol and 101 parts of triethylamine, and 200 parts of methyl isobutyl ketone was added thereto to form a solution. To this solution was added dropwise 78.4 parts of methacryloyl chloride (1.5 male based on 2-methyl-2-adamantanol). The solution was stirred at room temperature for about 10 hours. After 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-methyl-2-adamantyl methacrylate represented by the following formula in 75% yield:

후처리

  1. additionwas added
  2. customto form a solution
  3. filtrationAfter filtration
  4. washthe organic layer was washed with 5% aqueous sodium hydrogen carbonate solution
  5. washwashed twice with water
  6. concentrationThe organic layer was concentrated
  7. distillationdistilled under reduced pressure

출처 및 근거

ORD 기록
ord-4a437403d42f4442ae3524552564f443
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06548221B2

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