Trifluoroacetic anhydride → HCID 58201206、化合物

HRID 81695ノート

反応式

HRID 81695 の反応式
[Cl:1][C:2]1[C:3]([CH3:12])=[N+:4]([O-])[CH:5]=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9].FC(F)(F)C(OC(=O)C(F)(F)F)=[O:16]>ClCCl.C(Cl)(Cl)Cl>[Cl:1][C:2]1[C:3]([CH2:12][OH:16])=[N:4][CH:5]=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9]

参加物

5

反応物 2

HCID 9845Trifluoroacetic anhydrideHCID 143691543-Chloro-4-methoxy-2,5-dimethylpyridine 1-oxide

生成物 1

HCID 58201206HCID 58201206、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

The above 3-chloro-4-methoxy-2,5-dimethylpyridine 1-oxide (530 mg) was suspended in 15 ml of dichloromethane, and trifluoroacetic anhydride (0.39 ml) was then added to the suspension under cooling on ice. The resulting mixture was stirred at room temperature for 3 hours. The reaction solution was diluted with chloroform, and was then washed with a saturated sodium bicarbonate solution. The water layer was extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then distilled away, so as to obtain the title compound (521 mg) as an oily substance.

後処理

  1. temperatureunder cooling on ice
  2. washwas then washed with a saturated sodium bicarbonate solution
  3. extractionThe water layer was extracted with chloroform
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. distillationthe solvent was then distilled away

出典と根拠

ORDレコード
ord-831cdce3d3b94e2fbd5d876524cdd961
出典データセット
uspto-grants-2014_09
特許番号
US08846703B2

反応ノート

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