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

HRID 52136
ノート
印刷プレビュー

反応式

HRID 52136 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 21735183Dimethylformamide toluene
溶媒

実験手順

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 the 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.

後処理

  1. customThe mixture was reacted at 50-55° C. for 12 hours
  2. customAfter the completion of the 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

出典と根拠

ORDレコード
ord-d7f66b475d3b4a4dade481eadc6048e4
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05616581

反応ノート

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