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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 1382443
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HRID 1382443 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 129423121-Benzoyl-3-[1-(3-nitrobenzyl)piperid-4-yl]ureaHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b9ac26a008da4674ba57812adce70e3b
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04806552

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