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Methyl iodide → 4H-1,2,4-Triazole, 4-methyl-3-(methylthio)-5-(2-naphthalenyl)-

HRID 257162
ノート
印刷プレビュー

反応式

HRID 257162 の反応式
[CH3:1][N:2]1[C:6]([C:7]2[CH:16]=[CH:15][C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH:8]=2)=[N:5][NH:4][C:3]1=[S:17].[C:18]([O-])([O-])=O.[K+].[K+].CI>CC(C)=O>[CH3:1][N:2]1[C:3]([S:17][CH3:18])=[N:4][N:5]=[C:6]1[C:7]1[CH:16]=[CH:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 10243410HCID 10243410、化合物

生成物 1

HCID 30879994H-1,2,4-Triazole, 4-methyl-3-(methylthio)-5-(2-naphthalenyl)-

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 2,4-dihydro-4-methyl-5-(2-naphthyl)-3H-1,2,4-triazole-3-thione (5.26 g, 2.18×10-2 mole), K2CO3 (3.01 g, 2.18×10-2 mole), methyl iodide (1.5 ml, 2.4×10-2 mole), and acetone (65 ml) was stirred and warmed to reflux. After refluxing overnight, the solvent was evaporated at reduced pressure and the concentrate was treated with water. The aqueous mixture was extracted with EtOAc three times. The EtOAc extracts were combined, washed with saturated aqueous NaCl, and dried over anhydrous Na2SO4. The drying agent was removed by filtration and the filtrate was evaporated at reduced pressure to yield the desired product. Crystallization from Et0Ac afforded colorless plates, Mp 177°-179° C.

後処理

  1. temperaturewarmed to reflux
  2. temperatureAfter refluxing overnight
  3. customthe solvent was evaporated at reduced pressure
  4. additionthe concentrate was treated with water
  5. extractionThe aqueous mixture was extracted with EtOAc three times
  6. washwashed with saturated aqueous NaCl
  7. dry with materialdried over anhydrous Na2SO4
  8. customThe drying agent was removed by filtration
  9. customthe filtrate was evaporated at reduced pressure

出典と根拠

ORDレコード
ord-ce97e7cfceea460b86c31f1ce201a7bc
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05260450

反応ノート

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