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

HRID 743279노트

반응식

HRID 743279 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][CH2:32][O:33][CH3:34])[CH:26]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[CH3:34][O:33][CH2:32][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 194238641-t-Butoxycarbonyl-4-(2-{2-[2-(3-methoxymethoxyphenyl)ethyl]phenoxy}ethyl)piperidineHCID 21226445Aluminium lithium hydride

생성물 1

HCID 194240154-(2-{2-[2-(3-Methoxymethoxyphenyl)ethyl]phenoxy}ethyl)-1-methylpiperidine수율 62.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Following a procedure similar to that described in Example 38, 1.40 g of 1-t-butoxycarbonyl-4-(2-{2-[2-(3-methoxymethoxyphenyl) ethyl]phenoxy }ethyl) piperidine [prepared as described in Example 55 (a) ] were reacted with 240 mg of lithium aluminum hydride dispersed in 30 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 710 mg of the title compound as a colorless 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-82e17f73b8e5421aa8e52c996a94ba1f
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

반응 노트

불러오는 중…