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

HRID 563449ノート

反応式

HRID 563449 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 579149951-(1'-Ethoxyethoxy)-3-methacryloyloxyadamantane収率 99%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 8028Tetrahydrofuran溶媒

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-b16c97d351ee49668f703146f841eec4
出典データセット
uspto-grants-2011_11
特許番号
US08067515B2

反応ノート

読み込み中…