HCID 23370065、化合物 → HCID 23370086、化合物

HRID 1901072ノート

反応式

HRID 1901072 の反応式
[N+:1]([C:4]1[CH:28]=[CH:27][CH:26]=[CH:25][C:5]=1[O:6][CH2:7][CH2:8][CH2:9][C:10]1[CH:15]=[C:14]([C:16]([CH3:19])([CH3:18])[CH3:17])[C:13]([OH:20])=[C:12]([C:21]([CH3:24])([CH3:23])[CH3:22])[CH:11]=1)([O-])=O>C(O)C.[Pd]>[NH2:1][C:4]1[CH:28]=[CH:27][CH:26]=[CH:25][C:5]=1[O:6][CH2:7][CH2:8][CH2:9][C:10]1[CH:15]=[C:14]([C:16]([CH3:17])([CH3:18])[CH3:19])[C:13]([OH:20])=[C:12]([C:21]([CH3:23])([CH3:22])[CH3:24])[CH:11]=1

参加物

4

反応物 1

HCID 23370065HCID 23370065、化合物

生成物 1

HCID 23370086HCID 23370086、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

To a suspension of 4-[3-(2-nitrophenoxy)propyl]-2,6-di-t-butylphenol (1.03 g) in ethanol (30 ml) was added a catalytic amount of 10% palladium/carbon to carry out catalytic reduction under 3-4 arms at 40° C. for 10 hrs. After filtering off the catalyst, the solvent was distilled off to give 4-[3-(2-aminophenoxy)propyl]-2,6-di-t-butylphenol. This compound was dissolved in dichloromethane (20 ml), to which diisopropylamine (0.75 ml) was added. Phenyl chloroformate (0.84 g) was added dropwise under ice-cooling. After stirring the mixture at room temperature overnight, the reaction solution was washed with water and then saturated saline and dried over anhydrous MgSO4. After distilling off the solvent, the residue was purified by a silica gel column chromatography (hexane:ethyl acetate=15:1) to give 1-(1-benzyl-4-piperidyl)-3-[2-[3-(3,5-di-t-butyl-4-hydroxyphenyl)propoxy]phenyl]urea (1.23 g, 97%).

後処理

  1. customat 40° C.
  2. customfor 10 hrs
  3. filtrationAfter filtering off the catalyst
  4. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-2159bd6e50144a619b8d0076cebf4f79
出典データセット
uspto-grants-1996_11
特許番号
US05576335

反応ノート

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