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

HRID 703132노트

반응식

HRID 703132 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 (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.

후처리

  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

출처 및 근거

ORD 기록
ord-e6e5be09a0784c51b19c0fd56a3ee25f
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04981863

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