Pyridine → Pentaerythritol, dibenzoate

HRID 132726

반응식

HRID 132726 반응식
[OH:1][CH2:2][C:3]([CH2:8][OH:9])([CH2:6][OH:7])[CH2:4][OH:5].N1C=C[CH:13]=[CH:12][CH:11]=1.[C:16](Cl)(=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[O:25]1[CH2:29][CH2:28][CH2:27][CH2:26]1>>[C:16]([O:1][CH2:2][C:3]([CH2:8][OH:9])([CH2:6][OH:7])[CH2:4][O:5][C:29](=[O:25])[C:28]1[CH:13]=[CH:12][CH:11]=[CH:26][CH:27]=1)(=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

참가 물질

5

반응물 4

HCID 1049PyridineHCID 7412Benzoyl chlorideHCID 8028TetrahydrofuranHCID 8285Pentaerythritol

생성물 1

HCID 3059456Pentaerythritol, dibenzoate수율 95%

실험 절차

To 0.05 mol pentaerythritol were added 50 ml tetrahydrofuran and 0.15 mol pyridine, then added 0.12 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. After removing solvent, the crude was purified by column chromatography to give 2,2-dihydroxymethyl-1,3-propandiol dibenzoate as a colorless viscous liquid, and the yield was 95%.

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. customAfter removing solvent
  8. customthe crude was purified by column chromatography

출처 및 근거

ORD 기록
ord-52660cd048234f9b9ea2218a321aeabe
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07388061B2

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