Water → HCID 131716563, 화합물

HRID 1885920노트

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HRID 1885920 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.[C:15](=[O:18])([O-:17])[O-:16].[K+].[K+].Cl[CH2:22][CH2:23][CH2:24][N:25]([CH2:30][CH2:31][CH2:32][CH3:33])[CH2:26][CH2:27][CH2:28][CH3:29].[OH2:34]>CS(C)=O>[C:2]([OH:1])(=[O:34])[C:15]([OH:17])=[O:18].[C:15]([OH:16])(=[O:18])[C:2]([OH:1])=[O:34].[CH2:30]([N:25]([CH2:26][CH2:27][CH2:28][CH3:29])[CH2:24][CH2:23][CH2:22][O:1][C:2]1[CH:3]=[CH:4][C:5]([S:8][C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)=[CH:6][CH:7]=1)[CH2:31][CH2:32][CH3:33]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 96084N-(3-Chloropropyl)dibutylamineHCID 150806694-(pyridin-4-ylsulfanyl)phenol

생성물 1

HCID 131716563HCID 131716563, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A solution of 0.014 mol of 4-(4-hydroxy-phenylthio)pyridine and 3 g of finely crushed anhydrous potassium carbonate in 50 ml of dimethylsulphoxide was placed under stirring for 30 min. To this medium 0.016 mol of 1-chloro-3-(di-n-butylamino) propane was added and the stirring was maintained at room-temperature for 24 hours. The reaction medium was poured into water and extracted with ethyl ether. The organic phase was washed with water, dried on sodium sulphate and filtered. After the solvent was evaporated off, an oil was provided which was purified by chromatography on a silica column (eluent: methanol). The required compound in free base form so obtained was then transformed into an oxalate by adding an ethereal solution of oxalic acid.

후처리

  1. temperaturethe stirring was maintained at room-temperature for 24 hours
  2. extractionextracted with ethyl ether
  3. washThe organic phase was washed with water
  4. customdried on sodium sulphate
  5. filtrationfiltered
  6. customAfter the solvent was evaporated off
  7. customan oil was provided which
  8. customwas purified by chromatography on a silica column (eluent: methanol)

출처 및 근거

ORD 기록
ord-8262a97410cf4f7ab70deb6e92c74ed9
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05147878

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