Pyridine → Pentaerythritol, dibenzoate

HRID 132726

反応式

HRID 132726 の反応式
[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

参加物

5

反応物 4

HCID 1049PyridineHCID 7412Benzoyl chlorideHCID 8028TetrahydrofuranHCID 8285Pentaerythritol

生成物 1

HCID 3059456Pentaerythritol, dibenzoate収率 95%

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-52660cd048234f9b9ea2218a321aeabe
出典データセット
uspto-grants-2008_06
特許番号
US07388061B2

関連ノート

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