Hydrogen Peroxide → 2-(4-(Methylsulfinyl)phenoxy)-5-nitrobenzonitrile

HRID 1155737

반응식

HRID 1155737 반응식
[CH3:1][S:2][C:3]1[CH:20]=[CH:19][C:6]([O:7][C:8]2[CH:15]=[CH:14][C:13]([N+:16]([O-:18])=[O:17])=[CH:12][C:9]=2[C:10]#[N:11])=[CH:5][CH:4]=1.[OH:21]O.O>C(O)(=O)C>[CH3:1][S:2]([C:3]1[CH:20]=[CH:19][C:6]([O:7][C:8]2[CH:15]=[CH:14][C:13]([N+:16]([O-:18])=[O:17])=[CH:12][C:9]=2[C:10]#[N:11])=[CH:5][CH:4]=1)=[O:21]

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 962WaterHCID 514855Benzonitrile, 2-(4-(methylthio)phenoxy)-5-nitro-

생성물 1

HCID 128507692-(4-(Methylsulfinyl)phenoxy)-5-nitrobenzonitrile수율 92.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

To a slurry of 10.0 g (0.0350 moles) of 2-(4-(methylthio)phenoxy)-5-nitrobenzonitrile in 100 ml of glacial acetic acid was added a solution of 4.0 g of aqueous 30 percent (30%) hydrogen peroxide (0.0350 moles) dissolved in 20 ml of glacial acetic acid over 5 minutes. The reaction mixture was stirred at room temperature for 16 hrs and heated at 50° C. for 3 hrs. The reaction mixture was poured into water and the product collected by filtration, washed well with water and dried to obtain 9.8 g of product (92.8% yield). Recrystallization from ethanol afforded purified 2-(4-(methylsulfinyl)phenoxy)-5-nitrobenzonitrile, mp 159°-160° C.

후처리

  1. temperatureheated at 50° C. for 3 hrs
  2. filtrationthe product collected by filtration
  3. washwashed well with water
  4. customdried

출처 및 근거

ORD 기록
ord-a4774990aa5446608801949b2560f01b
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04332820

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