Pyridine → 1,2-butandiol Dibenzoate

HRID 132707

반응식

HRID 132707 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 231259061,2-butandiol Dibenzoate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b78bc78a8a854a8a814d4a63cfdec3ef
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07388061B2

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