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

HRID 1199381노트

반응식

HRID 1199381 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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 (4.83 g, 2.24×10-2 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 leaving an oil which slowly crystallized. Crystallization from EtOAc/hexane gave a colorless solid: 3.7 g (68%), mp 95°-97° C.

후처리

  1. washwas then washed
  2. dry with materialAfter drying over anhydrous Na2SO4
  3. customthe CH2Cl2 was evaporated
  4. customleaving an oil which
  5. customslowly crystallized
  6. customCrystallization from EtOAc/hexane
  7. customgave a colorless solid

출처 및 근거

ORD 기록
ord-65160f6939574b2eb9f7239b5ad24beb
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04900743

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