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1-Benzoyl-3-[1-(3-nitrobenzyl)piperid-4-yl]urea → 1-Benzoyl-3-[1-(3-aminobenzyl)piperid-4-yl]urea

HRID 1284567
ノート
印刷プレビュー

反応式

HRID 1284567 の反応式
[C:1]([NH:9][C:10]([NH:12][CH:13]1[CH2:18][CH2:17][N:16]([CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-])=O)[CH:21]=2)[CH2:15][CH2:14]1)=[O:11])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H][H]>[Pd]>[C:1]([NH:9][C:10]([NH:12][CH:13]1[CH2:18][CH2:17][N:16]([CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([NH2:26])[CH:21]=2)[CH2:15][CH2:14]1)=[O:11])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 129423121-Benzoyl-3-[1-(3-nitrobenzyl)piperid-4-yl]ureaHCID 178418361HCID 178418361、化合物

生成物 1

HCID 129423061-Benzoyl-3-[1-(3-aminobenzyl)piperid-4-yl]urea収率 46.1%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

1-Benzoyl-3-[1-(3-nitrobenzyl)piperid-4-yl]urea 4.47 g (from Example 13) was hydrogenated with 5% Pd/C (0.5 g) at atmospheric pressure and room temperature until no more hydrogen was taken up. The catalyst was filtered and the filtrate evaporated. The residue was dissolved in water and basified with 0.880 ammonia. The precipitated solid was filtered, washed well with water, dried, treated with charcoal, and evaporated to give the title compound, (1.9 gms). This was recrystallised from ethanolic HCl to give the dihydrochloride salt, monohydrate, m.p. 194°-195° C.

後処理

  1. filtrationThe catalyst was filtered
  2. customthe filtrate evaporated
  3. dissolutionThe residue was dissolved in water and basified with 0.880 ammonia
  4. filtrationThe precipitated solid was filtered
  5. washwashed well with water
  6. customdried
  7. additiontreated with charcoal
  8. customevaporated

出典と根拠

ORDレコード
ord-968ee0bd57814100957c24ce155d0081
出典データセット
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04563466

反応ノート

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