Ethyl vinyl ether → 1-(1'-Ethoxyethoxy)-3-methacryloyloxyadamantane

HRID 2261503노트

반응식

HRID 2261503 반응식
[OH:1][C:2]12[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][C:4]([O:12][C:13](=[O:17])[C:14]([CH3:16])=[CH2:15])([CH2:5]3)[CH2:3]1)[CH2:9]2.[CH2:18]([O:20][CH:21]=[CH2:22])[CH3:19].C([O-])([O-])=O.[Na+].[Na+]>O1CCCC1.Cl>[CH2:18]([O:20][CH:21]([O:1][C:2]12[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][C:4]([O:12][C:13](=[O:17])[C:14]([CH3:16])=[CH2:15])([CH2:5]3)[CH2:3]1)[CH2:9]2)[CH3:22])[CH3:19]

참가 물질

6

반응물 3

HCID 8023Ethyl vinyl etherHCID 10340Sodium CarbonateHCID 118565233-Hydroxy-1-methacryloyloxyadamantane

생성물 1

HCID 579149951-(1'-Ethoxyethoxy)-3-methacryloyloxyadamantane수율 99%

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매HCID 8028Tetrahydrofuran용매

실험 절차

Under a nitrogen atmosphere, 23.6 g (0.1 mols) of 1-hydroxy-3-methacryloyloxyadamantane (HAMA) was dissolved in 100 ml of tetrahydrofuran (THF) and 21.6 g (0.3 mols) of vinyl ethyl ether and 0.1 ml (1 mmol) of hydrochloric acid were added, followed by stirring at room temperature for 3 days. The reaction solution was neutralized with an aqueous Na2CO3 solution added and, after phase separation, the upper layer was washed with water so as to adjust the pH to 7. MgSO4 was added and the solution was dehydrated and filtered, and then concentrated to dryness to obtain 30 g of 1-(1′-ethoxyethoxy)-3-methacryloyloxyadamantane (EEAM) (yield: 99%)

후처리

  1. additionadded
  2. customafter phase separation
  3. washthe upper layer was washed with water so as
  4. additionMgSO4 was added
  5. filtrationfiltered
  6. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-86a871b70cf3422697aeeb763f05c9a7
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07847045B2

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