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

HRID 2213795
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HRID 2213795 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-41b335943b404876b1afa76d6f443a06
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07105531B2

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