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Potassium Iodide → 2,3-dimethyl-4-(2-morpholinoethylthio)pyridine-N-oxide

HRID 1720043
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HRID 1720043 반응식
Cl[CH2:2][CH2:3][S:4][C:5]1[CH:10]=[CH:9][N+:8]([O-:11])=[C:7]([CH3:12])[C:6]=1[CH3:13].C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[NH:22]1[CH2:27][CH2:26][O:25][CH2:24][CH2:23]1>CN(C)C=O.C1(C)C=CC=CC=1>[CH3:12][C:7]1[C:6]([CH3:13])=[C:5]([S:4][CH2:3][CH2:2][N:22]2[CH2:27][CH2:26][O:25][CH2:24][CH2:23]2)[CH:10]=[CH:9][N+:8]=1[O-:11]
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참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 8083MorpholineHCID 11430Potassium CarbonateHCID 199630384-(2-Chloroethylthio)-2,3-dimethylpyridine-N-oxide

생성물 1

HCID 199631002,3-dimethyl-4-(2-morpholinoethylthio)pyridine-N-oxide

시약·촉매·용매 1

HCID 21735183Dimethylformamide toluene
용매

실험 절차

4-(2-Chloroethylthio)-2,3-dimethylpyridine-N-oxide (6 g) was dissolved in a mixed solution of dimethylformamide-toluene (1:1) and thereto were added potassium carbonate (4.3 g), potassium iodide (4.4 g) and morpholine (1.9 ml). The mixture was reacted at 50°-55° C. for 12 hours. After the completion of tile reaction, inorganic matters were filtered off and the solvent was distilled away. Water was added to the residue and the mixture was extracted with chloroform. After drying over anhydrous magnesium sulfate, the chloroform was distilled away and the obtained residue was purified by silica gel column chromatography to give 3.4 g of 2,3-dimethyl-4-(2-morpholinoethylthio)pyridine-N-oxide.

후처리

  1. customThe mixture was reacted at 50°-55° C. for 12 hours
  2. customAfter the completion of tile reaction, inorganic matters
  3. filtrationwere filtered off
  4. distillationthe solvent was distilled away
  5. additionWater was added to the residue
  6. extractionthe mixture was extracted with chloroform
  7. dry with materialAfter drying over anhydrous magnesium sulfate
  8. distillationthe chloroform was distilled away
  9. customthe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-cef6abebf1b745ee97d1567bab358ef1
출처 데이터셋
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05504082

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