Ammonia → 4-[4-(4-Pyridyl)piperazin-1-yl]anisole

HRID 743811

반응식

HRID 743811 반응식
[N:1]1([C:7]2[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl.Cl[C:17]1[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=1.N>O>[N:20]1[CH:21]=[CH:22][C:17]([N:4]2[CH2:3][CH2:2][N:1]([C:7]3[CH:8]=[CH:9][C:10]([O:13][CH3:14])=[CH:11][CH:12]=3)[CH2:6][CH2:5]2)=[CH:18][CH:19]=1

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 818524-Chloropyridine hydrochlorideHCID 2697221-(4-Methoxyphenyl)piperazine

생성물 1

HCID 149869024-[4-(4-Pyridyl)piperazin-1-yl]anisole수율 31%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4-(piperazin-1-yl)anisole (4.24 g) and 4-chloropyridine hydrochloride (3.35 g) were intimately mixed and heated at 160°-170° C. (bath temperature) for 7 minutes. The solid obtained on cooling was dissolved in water (75 ml) and the solution basified with aqueous ammonia. The solid precipitate was extracted into ethyl acetate and the organic extract washed with water, filtered through phase separating paper (Whatman 1PS) and evaporated. The residue was recrystallised from ethanol to give 4-[4(4-pyridyl)piperazin-1-yl]anisole (1.84 g) as a solid: m.p. 165°-167° C.; NMR (CDCl3) δ8.3(2H,d); 6.86(4H,m); 6.71(2H,d); 3.78(3H,s); 3.46(4H,m); 3.2(4H,m).

후처리

  1. temperatureheated at 160°-170° C. (bath temperature) for 7 minutes
  2. customThe solid obtained
  3. temperatureon cooling
  4. extractionThe solid precipitate was extracted into ethyl acetate
  5. extractionthe organic extract
  6. washwashed with water
  7. filtrationfiltered through phase
  8. customseparating paper (Whatman 1PS)
  9. customevaporated
  10. customThe residue was recrystallised from ethanol

출처 및 근거

ORD 기록
ord-6239960c48f94bdca5fe27a1f187c165
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556977

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