Trifluoroacetic acid → 2-Chloro-3-nitro-6-picoline-N-oxide

HRID 1440480노트

반응식

HRID 1440480 반응식
[Cl:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([CH3:11])[N:3]=1.FC(F)(F)C(O)=[O:15].C(OO)(=O)C>C(O)(=O)C>[Cl:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([CH3:11])[N+:3]=1[O-:15]

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 6585Peracetic AcidHCID 12682302-Chloro-6-methyl-3-nitropyridine

생성물 1

HCID 194174682-Chloro-3-nitro-6-picoline-N-oxide

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

2-Chloro-3-nitro-6-picoline (2 g, 11.6 mmol) was added to an ice cooled mixture of trifluoroacetic acid (6 mL) and 30% peracetic acid in acetic acid (6 mL). The mixture was allowed to warm to room temperature over 30 minutes and was heated in a 60° C. oil bath for 5 hours. The mixture was partitioned between methylene chloride (100 mL) and water (50 mL). The pH was adjusted to 8 with 2.5 N sodium hydroxide and the aqueous layer was extracted with more methylene chloride (2×50 mL). The combined methylene chloride layers were dried with magnesium sulfate, filtered and evaporated to give the title compound as a white solid (1.6g).

후처리

  1. temperaturecooled
  2. temperaturewas heated in a 60° C. oil bath for 5 hours
  3. customThe mixture was partitioned between methylene chloride (100 mL) and water (50 mL)
  4. extractionthe aqueous layer was extracted with more methylene chloride (2×50 mL)
  5. dry with materialThe combined methylene chloride layers were dried with magnesium sulfate
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-40fd3cb602504fc4959be8ccb8dff417
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05498777

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