m-Chloroperbenzoic acid → 3-(2-Fluorophenyl)-5-(methanesulfinyl)-4-methyl-4H-1,2,4-triazole

HRID 703132ノート

反応式

HRID 703132 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[N:12]([CH3:13])[C:11]([S:14][CH3:15])=[N:10][N:9]=1.ClC1C=C(C=CC=1)C(OO)=[O:21]>C(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[N:12]([CH3:13])[C:11]([S:14]([CH3:15])=[O:21])=[N:10][N:9]=1

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 30879983-(2-Fluorophenyl)-4-methyl-5-(methylsulfanyl)-4H-1,2,4-triazole

生成物 1

HCID 30880003-(2-Fluorophenyl)-5-(methanesulfinyl)-4-methyl-4H-1,2,4-triazole

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred, 0° C., solution of 3-(2-fluorophenyl)-4-methyl-5-methylthio-4H-1,2,4-triazole (5.0 g, 2.2×10-2 mole) and CH2Cl2 (125 ml) was added portionwise m-chloroperoxybenzoic acid (12.1 g, 5.6×10-2 mole, 80% active MCPBA). After stirring overnight at room temperature, the reaction was diluted with CH2Cl2 until homogeneous and was then washed in turn twice with saturated aqueous NaHCO3 and once with saturated aqueous NaCl. After drying over anhydrous Na2SO4, the CH2Cl2 was evaporated at reduced pressure leaving a solid which was purified by chromatography and subsequent crystallization from EtOAc/hexane giving colorless matted needles: 3.6 (63%), mp 128°-130° C.

後処理

  1. washwas then washed
  2. dry with materialAfter drying over anhydrous Na2SO4
  3. customthe CH2Cl2 was evaporated at reduced pressure
  4. customleaving a solid which
  5. customwas purified by chromatography and subsequent crystallization from EtOAc/hexane giving colorless matted needles

出典と根拠

ORDレコード
ord-e6e5be09a0784c51b19c0fd56a3ee25f
出典データセット
uspto-grants-1991_01
特許番号
US04981863

反応ノート

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