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Acetic Anhydride → 3-[p-[3-(2-Acetoxyethyl)oxy-2-methylpropionyl]benzyl]pyridine

HRID 569161
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HRID 569161 반응식
[OH:1][CH2:2][CH2:3][O:4][CH2:5][CH:6]([CH3:22])[C:7]([C:9]1[CH:21]=[CH:20][C:12]([CH2:13][C:14]2[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=2)=[CH:11][CH:10]=1)=[O:8].[C:23](OC(=O)C)(=[O:25])[CH3:24]>N1C=CC=CC=1.C(OCC)(=O)C>[C:23]([O:1][CH2:2][CH2:3][O:4][CH2:5][CH:6]([CH3:22])[C:7]([C:9]1[CH:21]=[CH:20][C:12]([CH2:13][C:14]2[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=2)=[CH:11][CH:10]=1)=[O:8])(=[O:25])[CH3:24]
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참가 물질

5

반응물 2

HCID 7918Acetic AnhydrideHCID 137455213-[p-[3-(2-Hydroxyethyl)oxy-2-methylpropionyl]benzyl]pyridine

생성물 1

HCID 137455223-[p-[3-(2-Acetoxyethyl)oxy-2-methylpropionyl]benzyl]pyridine

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 8857Ethyl Acetate용매

실험 절차

In 3 ml of pyridine was dissolved 2.0 g of 3-[p-[3-(2-hydroxyethyl)oxy-2-methylpropionyl]benzyl]pyridine, and 0.76 ml of acetic anhydride was added to the resulting solution with ice-cooling, after which the resulting mixture was subjected to reaction at room temperature for 12 hours. The solvent was removed by distillation under reduced pressure, and the residue thus obtained was dissolved in 16 ml of ethyl acetate. The resulting solution was washed with 5 ml of water, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure to obtain crude oily 3-[p-[3-(2-acetoxyethyl)oxy-2-methylpropionyl]benzyl]pyridine. This was dissolved in 17 ml of ethanol.

후처리

  1. additionwas added to the resulting solution with ice-
  2. temperaturecooling
  3. customafter which the resulting mixture was subjected to reaction at room temperature for 12 hours
  4. customThe solvent was removed by distillation under reduced pressure
  5. customthe residue thus obtained
  6. washThe resulting solution was washed with 5 ml of water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe solvent was removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-7ef5a5dfd8af47d1a9d5356901b249ee
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04731370

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