m-Chloroperbenzoic acid → Hydrochloric Acid

HRID 1074931ノート

反応式

HRID 1074931 の反応式
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]

参加物

5

反応物 2

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

生成物 2

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-d05d22edf9d648a6a8262aa293f52237
出典データセット
uspto-grants-1983_07
特許番号
US04394509

反応ノート

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