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Aluminium lithium hydride → HCID 9860329, 화합물

HRID 227570
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인쇄 미리보기

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HRID 227570 반응식
C[O:2][C:3]([C@H:5]1[C@@H:10]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([Cl:18])[CH:12]=2)[CH2:9][CH2:8][N:7]([CH3:19])[CH2:6]1)=O.[H-].[H-].[H-].[H-].[Li+].[Al+3]>O1CCCC1>[CH3:19][N:7]1[CH2:8][CH2:9][C@H:10]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([Cl:18])[CH:12]=2)[C@H:5]([CH2:3][OH:2])[CH2:6]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 44429174(3S,4S)-methyl 4-(3,4-dichlorophenyl)-1-methylpiperidine-3-carboxylate

생성물 1

HCID 9860329HCID 9860329, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
-30 °C

실험 절차

A solution of (1) (5.0 g, 17 mmol) in tetrahydrofuran (50 ml) at −50° C. was added LiAlH4 (0.50 g, 13 mmol). Stirred at −30° C. for three hours, then quenched by addition of water and evaporated to a solid. The residue was dissolved in dichloromethane, dried with magnesium sulfate and evaporated to dryness. Yield 4.6 g of (3) (100%). Mp. 127-129° C.

후처리

  1. customquenched by addition of water
  2. customevaporated to a solid
  3. dissolutionThe residue was dissolved in dichloromethane
  4. dry with materialdried with magnesium sulfate
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-f6e2cd16ba6f44729086ded32bdbd24e
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07560562B2

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