1-t-Butoxycarbonyl-4-(2-{2-[2-(3-methoxyphenyl)ethyl]phenoxy}ethyl)piperidine → 4-(2-{2-[2-(3-Methoxyphenyl)ethyl]phenoxy}ethyl)-1-methylpiperidine

HRID 743276노트

반응식

HRID 743276 반응식
C(O[C:6]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[CH2:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([O:31][CH3:32])[CH:26]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[CH3:32][O:31][C:27]1[CH:26]=[C:25]([CH2:24][CH2:23][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[O:16][CH2:15][CH2:14][CH:11]2[CH2:10][CH2:9][N:8]([CH3:6])[CH2:13][CH2:12]2)[CH:30]=[CH:29][CH:28]=1

참가 물질

4

반응물 2

HCID 107655341-t-Butoxycarbonyl-4-(2-{2-[2-(3-methoxyphenyl)ethyl]phenoxy}ethyl)piperidineHCID 21226445Aluminium lithium hydride

생성물 1

HCID 105005754-(2-{2-[2-(3-Methoxyphenyl)ethyl]phenoxy}ethyl)-1-methylpiperidine수율 90.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Following a procedure similar to that described in Example 38, 2.15 g of 1-t-butoxycarbonyl-4-(2-{2-[2(3-methoxyphenyl)ethyl]phenoxy}ethyl)piperidine [prepared as described in Example 53 (a)] were reacted with 0.371 g of lithium aluminum hydride dispersed in 40 ml of tetrahydrofuran. The mixture was then worked up as described in Example 38, and the crude product thus obtained was purified by column chromatography through silica gel, using a 10:1 by volume mixture of methylene chloride and methanol as the eluent, to give 1.56 g (yield 90%) of 4-(2-{2-[2-(3-methoxyphenyl)ethyl]phenoxy}ethyl)-1-methylpiperidine as an oil.

후처리

  1. customthe crude product thus obtained
  2. customwas purified by column chromatography through silica gel
  3. additionby volume mixture of methylene chloride and methanol as the eluent

출처 및 근거

ORD 기록
ord-9fcd99ce3e80495da60236568643d767
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

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