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Oxygen → 3-ethyl-2,4-pentanediol Dibenzoate

HRID 132720
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HRID 132720 반응식
O=O.[CH2:3]([CH:5]([CH:9]([OH:11])[CH3:10])[CH:6]([OH:8])[CH3:7])[CH3:4].N1C=C[CH:15]=[CH:14][CH:13]=1.[C:18](Cl)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[CH2:27]1[CH2:31][O:30][CH2:29][CH2:28]1>N#N.O>[C:18]([O:8][CH:6]([CH:5]([CH2:3][CH3:4])[CH:9]([O:11][C:29](=[O:30])[C:28]1[CH:27]=[CH:31][CH:15]=[CH:14][CH:13]=1)[CH3:10])[CH3:7])(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 977OxygenHCID 1049PyridineHCID 7412Benzoyl chlorideHCID 8028TetrahydrofuranHCID 218678653-Ethyl-2,4-pentanediol

생성물 1

HCID 231259023-ethyl-2,4-pentanediol Dibenzoate

시약·촉매·용매 2

HCID 947
Nitrogen
용매
HCID 962Water용매

실험 절차

In N2 atmosphere free of water and oxygen, to a reactor were successively added 0.02 mol 3-ethyl-2,4-pentanediol, 20 ml THF, and 0.06 mol pyridine, then slowly added dropwise 0.05 mol benzoyl chloride. The reaction was heated refluxing for 8 hours, and allowed to continue at room temperature for further 12 hours. After the reaction was finished, the reaction mixture was filtered and the cake was washed with anhydrous ethyl ether for three times. The organic phase was completely washed with saturated saline, and dried over anhydrous sodium sulfate. Removing the solvent gave 5.1 g product.

후처리

  1. temperatureThe reaction was heated
  2. temperaturerefluxing for 8 hours
  3. filtrationthe reaction mixture was filtered
  4. washthe cake was washed with anhydrous ethyl ether for three times
  5. washThe organic phase was completely washed with saturated saline
  6. dry with materialdried over anhydrous sodium sulfate
  7. customRemoving the solvent

출처 및 근거

ORD 기록
ord-8f2f5528e6f94937a17744271aec00d2
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07388061B2

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