HCID 23370065, 화합물 → HCID 23370086, 화합물

HRID 1901072노트

반응식

HRID 1901072 반응식
[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

참가 물질

4

반응물 1

HCID 23370065HCID 23370065, 화합물

생성물 1

HCID 23370086HCID 23370086, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-2159bd6e50144a619b8d0076cebf4f79
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05576335

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