Aluminium lithium hydride → HCID 68766842, 화합물

HRID 1171598노트

반응식

HRID 1171598 반응식
[C:1]1([C@@H:7]([NH:9][C@H:10]2[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][C@H:11]2[C:23](OC)=[O:24])[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>CCOCC>[OH:24][CH2:23][C@H:11]1[C@@H:10]([NH:9][C@H:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH3:8])[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:20])([CH3:22])[CH3:21])=[O:17])[CH2:12]1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 58745527HCID 58745527, 화합물

생성물 1

HCID 68766842HCID 68766842, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a solution of (3R,4S)-1-tert-butyl 3-methyl 4-((S)-1-phenylethylamino)piperidine-1,3-dicarboxylate (47 g, 0.13 mol, see Ko, S. S. et al., WO 2002/002525 for preparation of the enantiomer of this compound) in anhydrous ether (500 mL) at 0° C. was added 1M-LAH (100 mL, 0.1 mol) dropwise, and the mixture was stirred at 015° C. for 3 h. The reaction was quenched with a portion-wise addition of Na2SO4.10H2O (excess) and stirring for 1 h at rt. It was filtered through Celite and the solvent was evaporated off to give (3R,4S)-tert-butyl 3-(hydroxymethyl)-4-((S)-1-phenylethylamino)piperidine-1-carboxylate (quantitative yield).

후처리

  1. customThe reaction was quenched with a portion-wise addition of Na2SO4.10H2O (excess)
  2. stirringstirring for 1 h at rt
  3. filtrationIt was filtered through Celite
  4. customthe solvent was evaporated off

출처 및 근거

ORD 기록
ord-bd7efb63d5ba442191f3971250b9f5ae
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07829571B2

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