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Sodium Acetate → 2-[(Acetyloxy)methyl]4-(2-chloroethoxy)-5-methoxybenzyl acetate

HRID 2213795
ノート
印刷プレビュー

反応式

HRID 2213795 の反応式
[Cl:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[C:9]([CH2:11]Cl)[C:8]([CH2:13]Cl)=[CH:7][C:6]=1[O:15][CH3:16].[C:17]([O-:20])(=[O:19])[CH3:18].[Na+]>C(O)(=O)C>[C:17]([O:20][CH2:13][C:8]1[CH:7]=[C:6]([O:15][CH3:16])[C:5]([O:4][CH2:3][CH2:2][Cl:1])=[CH:10][C:9]=1[CH2:11][O:20][C:17](=[O:19])[CH3:18])(=[O:19])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 517045Sodium AcetateHCID 117161401-(2-Chloroethoxy)-4,5-bis(chloromethyl)-2-methoxybenzene

生成物 1

HCID 115879752-[(Acetyloxy)methyl]4-(2-chloroethoxy)-5-methoxybenzyl acetate収率 86%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a solution of 5.67 g (0.020 mole) of 1-(2-chloroethoxy)-4,5-bis(chloromethyl)-2-methoxybenzene in 75 ml acetic acid is added a solution of 3.5 g of anhydrous sodium acetate in 100 ml acetic acid. This mixture is refluxed with stirring for 2 hours. Solids are removed by filtration and washed with acetic acid. The filtrate is evaporated to approximately 30 ml, then poured into water and extracted with ether. The organic phase is washed with aqueous sodium carbonate, water and brine. After drying over sodium sulfate, the solution is filtered and evaporated to give 5.69 g (86%) of 2-[(acetyloxy)methyl]-4-(2-chloroethoxy)-5-methoxybenzyl acetate as a white solid, m.p. 79–80° C.

後処理

  1. temperatureThis mixture is refluxed
  2. customSolids are removed by filtration
  3. washwashed with acetic acid
  4. customThe filtrate is evaporated to approximately 30 ml
  5. additionpoured into water
  6. extractionextracted with ether
  7. washThe organic phase is washed with aqueous sodium carbonate, water and brine
  8. dry with materialAfter drying over sodium sulfate
  9. filtrationthe solution is filtered
  10. customevaporated

出典と根拠

ORDレコード
ord-41b335943b404876b1afa76d6f443a06
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07105531B2

反応ノート

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