m-Chloroperbenzoic acid → Hydrochloric Acid

HRID 1074931노트

반응식

HRID 1074931 반응식
Cl.[F:2][C:3]([F:19])([F:18])[C:4]1[CH:5]=[C:6]([S:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)[CH:7]=[CH:8][CH:9]=1.[Cl:20]C1C=C(C=CC=1)C(OO)=[O:25]>C(Cl)Cl>[F:19][C:3]([F:2])([F:18])[C:4]1[CH:5]=[C:6]([S:10]([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)=[O:25])[CH:7]=[CH:8][CH:9]=1.[ClH:20]

참가 물질

5

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 129532902-({[3-(Trifluoromethyl)phenyl]sulfanyl}methyl)pyridine--hydrogen chloride (1/1)

생성물 2

HCID 313Hydrochloric Acid수율 419.3%HCID 127602352-{[3-(Trifluoromethyl)benzene-1-sulfinyl]methyl}pyridine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A stirred suspension of 2-(((3-trifluoromethylphenyl)thio)methylpyridine, hydrochloride (2.0 g) in methylene chloride (50 ml) at 0° C. was treated portionwise with m-chloroperoxybenzoic acid (1.5 g) over 1/2 hour. The mixture was allowed to warm to ambient temperature and the mixture was stirred a further 1/2 hour. The solution was washed with saturated Na2CO3 solution and water, dried (MgSO4) and evaporated. The residue was converted into the hydrochloride, in acetone with ethereal HCl solution, which was recrystallised from acetone-ether to give the title compound, hydrochloride (1.0 g) mp 135°-6° C. (Found: C,48.3; H,3.7; N,4.0 C13H10F3NOS.HCl requires C,48.4; H,3.45; N,4.35%).

후처리

  1. washThe solution was washed with saturated Na2CO3 solution and water
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customwas recrystallised from acetone-ether

출처 및 근거

ORD 기록
ord-d05d22edf9d648a6a8262aa293f52237
출처 데이터셋
uspto-grants-1983_07
특허 번호
US04394509

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