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Water → HCID 19088496, 화합물

HRID 1587870
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HRID 1587870 반응식
[CH2:1]([N:8]([C:10]([CH3:18])([CH3:17])[CH2:11][C:12](OCC)=[O:13])[CH3:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[CH2:1]([N:8]([C:10]([CH3:18])([CH3:17])[CH2:11][CH2:12][OH:13])[CH3:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 19088497HCID 19088497, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 19088496HCID 19088496, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of ethyl 3-(N-benzyl-N-methylamino)-3-methylbutanoate (23.6 g-see Preparation 9) in anhydrous tetrahydrofuran (100 ml) was added, dropwise, over 20 minutes to a stirred suspension of lithium aluminium hydride (7.2 g) in anhydrous tetrahydrofuran (300 ml). When the addition was complete, the mixture was stirred at room temperature for 3 hours. Water (7 ml) was carefully added dropwise followed by 15% aqueous sodium hydroxide (7 ml) and finally more water (20 ml). The resulting solid precipitate was filtered off and washed with ethyl acetate (3×50 ml). The filtrate and washings were combined and concentrated in vacuo to give the title compound as a colourless, mobile oil, yield 19.0 g.

후처리

  1. additionWhen the addition
  2. filtrationThe resulting solid precipitate was filtered off
  3. washwashed with ethyl acetate (3×50 ml)
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a7929a7d6ca148a2af88ee80951bb91b
출처 데이터셋
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05219871

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