Pyridine → 1,2-butandiol Dibenzoate

HRID 132707

反応式

HRID 132707 の反応式
[CH2:1]([OH:6])[CH:2]([OH:5])[CH2:3][CH3:4].[C:7](Cl)(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.N1C=C[CH:19]=[CH:18][CH:17]=1.[O:22]1[CH2:26][CH2:25][CH2:24][CH2:23]1>O>[C:7]([O:6][CH2:1][CH:2]([O:5][C:26](=[O:22])[C:25]1[CH:19]=[CH:18][CH:17]=[CH:23][CH:24]=1)[CH2:3][CH3:4])(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

6

反応物 4

HCID 1049PyridineHCID 7412Benzoyl chlorideHCID 8028TetrahydrofuranHCID 114291,2-Butanediol

生成物 1

HCID 231259061,2-butandiol Dibenzoate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To the reactor were added 1,2-butylene-glycol (2.5 g), benzoyl chloride (7.8 g), pyridine (8.8 g) and tetrahydrofuran (70 ml). The reactants was mixed and heated refluxing for 4 hours, then cooled to room temperature. Water was added to the reaction system until the inorganic phase was transparent. Organic phase was separated. Inorganic phase was extracted with ethyl ether. The combined organic phase was washed with water, dried over anhydrous sodium sulfate. After concentrated, 3.95 g product was separated. 1H-NMR: δ (ppm)1.0-1.1 (3H), 1.7-1.9(2H), 4.4-4.6(2H), 5.4-5.5(1H) and 7.4-8.2(10H).

後処理

  1. additionThe reactants was mixed
  2. temperatureheated
  3. temperaturerefluxing for 4 hours
  4. customOrganic phase was separated
  5. extractionInorganic phase was extracted with ethyl ether
  6. washThe combined organic phase was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationAfter concentrated
  9. custom3.95 g product was separated

出典と根拠

ORDレコード
ord-b78bc78a8a854a8a814d4a63cfdec3ef
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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