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1H-1,2,4-Triazole → HCID 20079600、化合物

HRID 1033737
ノート
印刷プレビュー

反応式

HRID 1033737 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1([C:12]([S:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=2)([CH3:14])[CH3:13])[CH2:11][O:10]1.[NH:25]1[CH:29]=[N:28][CH:27]=[N:26]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:10])([C:12]([S:15][CH2:16][C:17]1[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=1)([CH3:14])[CH3:13])[CH2:11][N:25]1[CH:29]=[N:28][CH:27]=[N:26]1
参加物反応条件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 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 19024387HCID 19024387、化合物

生成物 1

HCID 20079600HCID 20079600、化合物収率 94.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
105 °C

実験手順

A mixture of 64.0 g (182 mmol) of (-)-2-(2,4-difluorophenyl)-2-(1-((4-methoxyphenyl)methylthio)-1-methylethyl)oxirane, 25.1 g (364 mmol) of 1,2,4-triazole, 50.3 g (364 mmol) of potassium carbonate, and 910 ml of DMF was stirred at 105° C. for 17 hours. After allowing the mixture to cool, the solvent was removed by distillation under reduced pressure, and to the residue were added dichloromethane and water. The organic layer was separated, washed with a saturated sodium chloride aqueous solution, and dried. The solvent was removed by distillation under reduced pressure, and the residue was purified by column chromatography using a mixed solvent of chloroform and methanol (30:1) as an eluent. The solvent was removed by distillation under reduced pressure to obtain 72.0 g (94%) of (+)-2-(2,4-difluorophenyl)-3-((4-methoxyphenyl)methylthio)-3-methyl-1-(1H-1,2,4-triazol-1-yl)butan-2-ol as a pale yellow oily substance.

後処理

  1. temperatureto cool
  2. customthe solvent was removed by distillation under reduced pressure
  3. additionto the residue were added dichloromethane and water
  4. customThe organic layer was separated
  5. washwashed with a saturated sodium chloride aqueous solution
  6. customdried
  7. customThe solvent was removed by distillation under reduced pressure
  8. customthe residue was purified by column chromatography
  9. customThe solvent was removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-af36e9d1059d41739aede6190f4d7d40
出典データセット
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05312815

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート