Cesium carbonate → 4-Pyridyloxyundecan-1-ol

HRID 278286

반응식

HRID 278286 반응식
[OH:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][OH:26]>CN(C=O)C>[N:5]1[CH:6]=[CH:7][C:2]([O:1][CH:25]([OH:26])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH3:15])=[CH:3][CH:4]=1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 7416311-Bromo-1-undecanolHCID 178418642HCID 178418642, 화합물

생성물 1

HCID 226277984-Pyridyloxyundecan-1-ol수율 22%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
90 °C

실험 절차

The compound 4-pyridyloxyundecan-1-ol was prepared as follows: To a solution of 4-hydroxy-pyridine (5.71 g, 60 mmol) in DMF (150 cm3) was added cesium carbonate (19.56 g, 60 mmol). The mixture was heated to 90° C. for 5 mins then 11-bromoundecanol (12.56 g, 50 mmol) was added and the mixture heated to reflux temperature (125° C.) for 15 hours. After cooling, the contents of the flask were poured into rapidly stirring distilled water (800 cm3). A pale yellow precipitate formed which was filtered and dried (in air). Recrystallization from hexane gave white crystals of 4-pyridyloxyundecan-1-ol (2.9 g, 22%).

후처리

  1. customThe compound 4-pyridyloxyundecan-1-ol was prepared
  2. temperaturethe mixture heated
  3. temperatureto reflux temperature (125° C.) for 15 hours
  4. temperatureAfter cooling
  5. additionthe contents of the flask were poured
  6. distillationdistilled water (800 cm3)
  7. customA pale yellow precipitate formed which
  8. filtrationwas filtered
  9. customdried (in air)
  10. customRecrystallization from hexane

출처 및 근거

ORD 기록
ord-b20d2e813885471983fcc0bca3358792
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06359056B1

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