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

HRID 1586930노트

반응식

HRID 1586930 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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%

후처리

  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

출처 및 근거

ORD 기록
ord-de3a327cf06b4ad4805939d7cc188dc7
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05216134

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