Phosphorus tribromide → 6,6'-Dimethyl-4-ethoxy-2,2'-bipyridine

HRID 1586930ノート

反応式

HRID 1586930 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([O:16][CH2:17][CH3:18])[CH:5]=[C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[N:10]=2)[N+:7]=1[O-].P(Br)(Br)Br>C(Cl)(Cl)Cl>[CH3:1][C:2]1[N:7]=[C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[N:10]=2)[CH:5]=[C:4]([O:16][CH2:17][CH3:18])[CH:3]=1

参加物

4

反応物 2

HCID 24614Phosphorus tribromideHCID 149751976,6'-Dimethyl-4-ethoxy-2,2'-bipyridine-N-oxide

生成物 1

HCID 149751986,6'-Dimethyl-4-ethoxy-2,2'-bipyridine収率 69%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

6,6'-Dimethyl-4-ethoxy-2,2'-bipyridine-N-oxide (21) (0.96 g, 3.93 mmoles) was dissolved in chloroform (34 ml). After addition of phosphorus tribromide (3.0 ml) the mixture was refluxed for 1.5 hours. The solution was poured on ice, some chloroform was added and the phases were separated. The chloroform phase was extracted with water. The aqueous phases were combined, made alkaline with sodium hydroxide solution, and extracted with chloroform. Evaporation of the organic phase followed by silica gel chromatography yielded pure title product. Yield: 69%

後処理

  1. temperaturewas refluxed for 1.5 hours
  2. additionThe solution was poured on ice
  3. customthe phases were separated
  4. extractionThe chloroform phase was extracted with water
  5. extractionextracted with chloroform
  6. customEvaporation of the organic phase

出典と根拠

ORDレコード
ord-de3a327cf06b4ad4805939d7cc188dc7
出典データセット
uspto-grants-1993_06
特許番号
US05216134

反応ノート

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