4-(Aminomethyl)piperidine → 4-(2,3,5,6-Tetrachloropyridin-4-ylaminomethyl)pyridine

HRID 1957522노트

반응식

HRID 1957522 반응식
[N+:1]([C:4]1[C:9]([Cl:10])=[C:8]([Cl:11])[N:7]=[C:6]([Cl:12])[C:5]=1[Cl:13])([O-])=O.N[CH2:15][CH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1>O1CCOCC1>[Cl:11][C:8]1[C:9]([Cl:10])=[C:4]([NH:1][CH2:15][C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)[C:5]([Cl:13])=[C:6]([Cl:12])[N:7]=1

참가 물질

4

반응물 2

HCID 235274-(Aminomethyl)piperidineHCID 152291672,3,5,6-Tetrachloro-4-nitropyridine

생성물 1

HCID 190680884-(2,3,5,6-Tetrachloropyridin-4-ylaminomethyl)pyridine수율 24.3%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

1 g 4-nitro-2,3,5,6-tetrachloropyridine, 0.65 g 4-aminomethylpiperidine and 20 ml absolute dioxane were stirred for 1 hour at room temperature. Subsequently the dioxane was removed by distillation, the residue was admixed with water, separated from undissolved material and the aqueous phase was extracted several times with dichloromethane. After drying and evaporating the solvent, the residue can be crystallized from a small amount of diethyl ether. 0.3 g 4-(2,3,5,6-tetrachloropyridin-4-ylaminomethyl)pyridine is obtained as colourless crystals. TLC (mobile solvent: toluene/dioxane/water 90:20:0.2), Rf=0.8.

후처리

  1. customSubsequently the dioxane was removed by distillation
  2. customseparated from undissolved material
  3. extractionthe aqueous phase was extracted several times with dichloromethane
  4. customAfter drying
  5. customevaporating the solvent
  6. customthe residue can be crystallized from a small amount of diethyl ether

출처 및 근거

ORD 기록
ord-84fabf165bc542ec84c65cb7c38a9b47
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05786371

반응 노트

불러오는 중…