HCID 20569917、化合物 → N-Butyl-N'-piperidin-4-ylurea

HRID 1577841ノート

反応式

HRID 1577841 の反応式
Cl.[CH2:2]([NH:6][C:7](=[O:15])[NH:8][C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=1)[CH2:3][CH2:4][CH3:5].[H][H]>C(O)C.O.[Rh]>[CH2:2]([NH:6][C:7](=[O:15])[NH:8][CH:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1)[CH2:3][CH2:4][CH3:5]

参加物

5

反応物 2

HCID 20569917HCID 20569917、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 12608579N-Butyl-N'-piperidin-4-ylurea収率 19.4%

試薬・触媒・溶媒 2

HCID 23948Rhodium触媒HCID 19096565Water ethanol溶媒

実験手順

A solution of 3-n-butyl-1-(4-pyridyl)urea hydrochloride (37.4 g) in ethanol-water (1:1, 400 ml) containing 5% rhodium/alumina catalyst (10 g) was hydrogenated (50°, 750 psi) until no further uptake of hydrogen occurred. The catalyst was then removed by filtration and the solvent evaporated to leave an oil which partially solidified on storage at 0°. The solid was separated, treated with base, extracted with chloroform/n-butanol, the extracts evaporated and the residue recrystallized twice from ethyl acetate to give 3-n-butyl-1-(4-piperidyl)urea, (6.3 g), m.p. 132°-134°.

後処理

  1. custom(50°, 750 psi)
  2. customThe catalyst was then removed by filtration
  3. customthe solvent evaporated
  4. customto leave an oil which
  5. custompartially solidified on storage at 0°
  6. customThe solid was separated
  7. additiontreated with base
  8. extractionextracted with chloroform/n-butanol
  9. customthe extracts evaporated
  10. customthe residue recrystallized twice from ethyl acetate

出典と根拠

ORDレコード
ord-98bd7d0e70a547579e4503920b53fe44
出典データセット
uspto-grants-1981_09
特許番号
US04289772

反応ノート

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