Hydrogen Peroxide → 2-Chloro-4-methylpyridine 1-oxide

HRID 1039081

반응식

HRID 1039081 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N:3]=1.OO.C([O-])([O-])=[O:12].[Na+].[Na+]>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N+:3]=1[O-:12]

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 10340Sodium CarbonateHCID 772482-Chloro-4-methylpyridine

생성물 1

HCID 124874842-Chloro-4-methylpyridine 1-oxide

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
65 °C

실험 절차

2-chloro-4-methylpyridine (10 g, 80 mmol) was dissolved in acetic acid (100 ml). Hydrogen peroxide (31%, 86.8 g, 80.7 ml, 790 mmol)) was added in 4 portions and the solution stirred under nitrogen at 65° C. for 18 hours. The mixture was poured into ice water (300 ml), and solid Na2CO3 added until the solution was alkaline. The mixture was extracted with DCM (3×300 ml), the organic fractions combined, washed with sodium thiosulfate (1M, 100 ml), brine, dried over Na2SO4, and the volatiles removed in vacuum to give the titled compound.

후처리

  1. additionadded until the solution
  2. extractionThe mixture was extracted with DCM (3×300 ml)
  3. washwashed with sodium thiosulfate (1M, 100 ml), brine
  4. dry with materialdried over Na2SO4
  5. customthe volatiles removed in vacuum

출처 및 근거

ORD 기록
ord-6a615a75ed284508a0b89c6529a24c42
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552022B2

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