1-Methyl-1-(4-pyridylmethyl)-3-phenylurea → 1-Methyl-1-(4-piperidylmethyl)-3-cyclohexylurea

HRID 1164514ノート

反応式

HRID 1164514 の反応式
[CH3:1][N:2]([CH2:12][C:13]1[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=1)[C:3]([NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:4].[H][H]>C(O)(=O)C.[Pt]=O>[CH3:1][N:2]([CH2:12][CH:13]1[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]1)[C:3]([NH:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1)=[O:4]

参加物

5

反応物 2

HCID 205111981-Methyl-1-(4-pyridylmethyl)-3-phenylureaHCID 178418361HCID 178418361、化合物

生成物 1

HCID 205111921-Methyl-1-(4-piperidylmethyl)-3-cyclohexylurea収率 54.4%

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 176Acetic Acid溶媒

実験手順

1-Methyl-1-(4-pyridylmethyl)-3-phenylurea (7.0 g) in glacial acetic acid (50 ml) was hydrogenated over platinum oxide at 60°/60 p.s.i. until uptake of hydrogen ceased. The catalyst was removed by filtration and the filtrate evaporated in vacuo. The resultant oil was basified with 5 N NaOH (to pH 12) and extracted with chloroform (2×50 ml). The combined extracts were dried (MgSO4) and evaporated with chloroform (2×50 ml). The combined extracts were dried (MgSO4) and evaporated to give 1-methyl-1-(4-piperidylmethyl)-3-cyclohexylurea as an oil (4.0 g). The n.m.r. and mass spectra were compatible with the required structure.

後処理

  1. customThe catalyst was removed by filtration
  2. customthe filtrate evaporated in vacuo
  3. extractionextracted with chloroform (2×50 ml)
  4. dry with materialThe combined extracts were dried (MgSO4)
  5. customevaporated with chloroform (2×50 ml)
  6. dry with materialThe combined extracts were dried (MgSO4)
  7. customevaporated

出典と根拠

ORDレコード
ord-28a56f0610ff4e2599e3656291c640c7
出典データセット
uspto-grants-1983_01
特許番号
US04370328

反応ノート

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