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

HRID 408448
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HRID 408448 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 (20 mmol) of 36 in 75 mL of acetic acid was added a solution of 3.5 g of anhydrous sodium acetate (42.7 mmol) in 100 mL of acetic acid. This mixture was refluxed with stirring for 2 h. Solids were removed by filtration and washed with acetic acid. The filtrate was evaporated to approximately 30 mL, then poured into water and extracted with ether. The organic phase was washed with aqueous sodium carbonate, water, and brine. After drying over sodium sulfate, the solution was filtered and evaporated to give 5.69 g (86%) of 2-[(acetyloxy)methyl]-4-(2-chloroethoxy)-5-methoxybenzyl acetate (37) as a white solid, mp 79-80° C.

후처리

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

출처 및 근거

ORD 기록
ord-d8574a2add784f29906a8129f6c6f30e
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08759339B2

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