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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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m-Chloroperbenzoic acid → HCID 18377464, 화합물

HRID 1255902
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HRID 1255902 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([CH3:11])([CH3:10])[CH3:9])[CH:5]=[CH:4][N:3]=1.C1C=C(Cl)C=C(C(OO)=[O:20])C=1.S(=O)(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([CH3:11])([CH3:10])[CH3:9])[CH:5]=[CH:4][N+:3]=1[O-:20]
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참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acidHCID 516919Sodium BisulfateHCID 573459814-tert-Butyl-2-chloropyridine

생성물 1

HCID 18377464HCID 18377464, 화합물수율 90%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

2-Chloro-4-t-butylpyridine (5.0 g, 30 mmol) was dissolved in chloroform (75 mL), treated with MCPBA, ca. 75% (8.3 g, 36 mmol, 1.2 equivalents) and heated to reflux for 19 h. The mixture was stirred with sodium bisulfate solution until testing with starch-iodide paper indicated consumption of oxidant. The pH was adjusted to 7 with saturated aqueous NaHCO3 solution, the phases separated and the aqueous phase extracted once with CH2Cl2. The organic phases were pooled and washed twice with H2O, once with brine, dried (Na2SO4) and concentrated in vacuo to afford 2-chloro-4-t-butylpyridine-N-oxide (5.0 g, 90%), which crystallized to long white needles on standing.

후처리

  1. temperatureheated
  2. temperatureto reflux for 19 h
  3. customconsumption of oxidant
  4. customthe phases separated
  5. extractionthe aqueous phase extracted once with CH2Cl2
  6. washwashed twice with H2O, once with brine
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-dcfbd2ad85bd4338b4ffda44114106da
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461164B2

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