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Methacrylic Acid → (2-Adamantyloxymethyl)methacrylate

HRID 1716170
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HRID 1716170 반응식
[C:1]([OH:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].C(N(CC)CC)C.Cl[CH2:15][O:16][CH:17]1[CH:24]2[CH2:25][CH:20]3[CH2:21][CH:22]([CH2:26][CH:18]1[CH2:19]3)[CH2:23]2>O1CCCC1>[CH:18]12[CH2:26][CH:22]3[CH2:21][CH:20]([CH2:25][CH:24]([CH2:23]3)[CH:17]1[O:16][CH2:15][O:5][C:1](=[O:6])[C:2]([CH3:4])=[CH2:3])[CH2:19]2
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참가 물질

5

반응물 3

HCID 4093Methacrylic AcidHCID 8471TriethylamineHCID 10932491HCID 10932491, 화합물

생성물 1

HCID 23150858(2-Adamantyloxymethyl)methacrylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

6.9 g of methacrylic acid was dissolved in 200 ml of tetrahydrofuran, and 8.0 g of triethylamine was added. Following stirring at room temperature, a solution containing 15 g of 2-adamantyl chloromethyl ether dissolved in 100 ml of tetrahydrofuran was added dropwise to the reaction solution. Following stirring for 12 hours at room temperature, the precipitated salt was removed by filtration. The solvent was removed from the remaining filtrate by evaporation, the residue was dissolved in 200 ml of ethyl acetate, and following washing with pure water (100 ml×3), the solvent was removed by evaporation. The residue was then allowed to stand under ice cooling, thereby yielding a white solid.

후처리

  1. additionwas added dropwise to the reaction solution
  2. stirringFollowing stirring for 12 hours at room temperature
  3. customthe precipitated salt was removed by filtration
  4. customThe solvent was removed from the remaining filtrate by evaporation
  5. dissolutionthe residue was dissolved in 200 ml of ethyl acetate
  6. washfollowing washing with pure water (100 ml×3)
  7. customthe solvent was removed by evaporation
  8. customyielding a white solid

출처 및 근거

ORD 기록
ord-5c70ff849142413b982041e4b5459fee
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07803512B2

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