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Sodium Hydroxide → HCID 68814812, 화합물

HRID 730026
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HRID 730026 반응식
[C:1]1([C:11](=[O:13])[CH3:12])[C:10]2[C:4]([CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)=[CH:3][CH:2]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+].S([O-])([O-])(=O)=O.[Mg+2]>C1COCC1>[C:1]1([CH:11]([OH:13])[CH3:12])[C:10]2[C:4]([CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 24083Sulfuric acid magnesium salt (1:1)HCID 111828801-AcetylazuleneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 68814812HCID 68814812, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1-(Azulen-1-yl)ethanone (13.0 g) prepared according to a method described in the literature (Mori et al., J. Heterocycl. Chem., Vol. 33, 1996, pp. 841-846) was dissolved in dehydrated THF (380 mL), and stirried with cooling on ice under nitrogen atmosphere. This reaction mixture was carefully added with lithium aluminum hydride (1.45 g, Wako Pure Chemical Industries), and stirried with cooling on ice for 1 hour. The reaction mixture was carefully added with 2 N aqueous sodium hydroxide with cooling on ice and stirring. The reaction mixture was added with anhydrous magnesium sulfate, and stirred, then the solid was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was used for the subsequent reaction as it was.

후처리

  1. temperaturewith cooling on ice under nitrogen atmosphere
  2. temperaturewith cooling on ice for 1 hour
  3. temperaturewith cooling on ice
  4. stirringstirred
  5. customthe solid was removed by filtration
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe residue was used for the subsequent reaction as it

출처 및 근거

ORD 기록
ord-ef4dd3500e6a41859c66357fde23d801
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582658B2

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