Pyridine → 2-Methyl-2,4-pentanediol dibenzoate

HRID 132711

반응식

HRID 132711 반응식
[CH3:1][C:2]([OH:8])([CH2:4][CH:5]([OH:7])[CH3:6])[CH3:3].N1C=C[CH:12]=[CH:11][CH:10]=1.[C:15](Cl)(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[O:24]1[CH2:28][CH2:27][CH2:26][CH2:25]1>>[C:15]([O:8][C:2]([CH3:3])([CH2:4][CH:5]([O:7][C:28](=[O:24])[C:27]1[CH:12]=[CH:11][CH:10]=[CH:25][CH:26]=1)[CH3:6])[CH3:1])(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

5

반응물 4

HCID 1049PyridineHCID 7412Benzoyl chlorideHCID 7870Hexylene GlycolHCID 8028Tetrahydrofuran

생성물 1

HCID 193919182-Methyl-2,4-pentanediol dibenzoate수율 88%

실험 절차

To 0.03 mol 2-methyl-2,4-pentanediol were added 30 ml tetrahydrofuran and 0.09 mol pyridine, then added 0.075 mol benzoyl chloride with stirring. The reaction was heated refluxing for 4 hours, cooled and added 20 ml saturated saline. The reaction mixture was extracted with ethyl acetate, and the extract was dried over anhydrous sodium sulfate, filtered. After removing solvent, the crude was purified by column chromatography to give 2-methyl-2,4-pentanediol dibenzoate as a colorless liquid, and the yield was 88%.

후처리

  1. temperatureThe reaction was heated
  2. temperaturerefluxing for 4 hours
  3. temperaturecooled
  4. additionadded 20 ml saturated saline
  5. extractionThe reaction mixture was extracted with ethyl acetate
  6. dry with materialthe extract was dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. customAfter removing solvent
  9. customthe crude was purified by column chromatography

출처 및 근거

ORD 기록
ord-e577ef99881a4f6d9be847a415bff470
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07388061B2

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