1H-1,2,4-Triazole → 1-(4-Chlorophenyl)-3-(1,2,4-triazol-1-yl)-2-propanol

HRID 2107065

反応式

HRID 2107065 の反応式
C(=O)([O-])[O-].[K+].[K+].[NH:7]1[CH:11]=[N:10][CH:9]=[N:8]1.[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][CH:20]2[O:22][CH2:21]2)=[CH:15][CH:14]=1>C(#N)C>[Cl:12][C:13]1[CH:14]=[CH:15][C:16]([CH2:19][CH:20]([OH:22])[CH2:21][N:7]2[CH:11]=[N:10][CH:9]=[N:8]2)=[CH:17][CH:18]=1

参加物

5

反応物 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 148012Oxirane, 2-((4-chlorophenyl)methyl)-

生成物 1

HCID 230476741-(4-Chlorophenyl)-3-(1,2,4-triazol-1-yl)-2-propanol

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of potassium carbonate (8.14 g) and 1,2,4-triazole (8.14 g) in acetonitrile (100 ml) was added 1-(4-chlorophenyl)-2,3-epoxypropane (9.0 g), and the resulting suspension was heated to 70° for 4.5 h. The excess acetonitrile was evaporated under reduced pressure, and the residue was partitioned between ethyl acetate and water. The organic layer was separated, washed with water and dried, and the solvent was evaporated to give a colourless oil. Purification by column chromatography on silica, eluting with chloroform/methanol, 95:5 by volume, gave 1-(4-chlorophenyl)-3-(1,2,4-triazol-1-yl)-2-propanol as a colourless oil which crystallised on standing, m.p. 104°-6°.

後処理

  1. temperaturethe resulting suspension was heated to 70° for 4.5 h
  2. customThe excess acetonitrile was evaporated under reduced pressure
  3. customthe residue was partitioned between ethyl acetate and water
  4. customThe organic layer was separated
  5. washwashed with water
  6. customdried
  7. customthe solvent was evaporated
  8. customto give a colourless oil
  9. customPurification by column chromatography on silica
  10. washeluting with chloroform/methanol, 95:5 by volume

出典と根拠

ORDレコード
ord-84fc1dc50ae94feab1ac728387b645d9
出典データセット
uspto-grants-1990_06
特許番号
US04933357

関連ノート

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