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

HRID 2207

反応式

HRID 2207 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-61aad68a3b1947e1aaa4cb73733b890c
出典データセット
uspto-grants-1998_03
特許番号
US05728701

関連ノート

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