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Sulfuric Acid → 6,6-Dimethylhepta-2,4-dienal

HRID 851168
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HRID 851168 반응식
C[O:2][CH:3]=[CH:4][C:5]#[CH:6].[C:7]([Mg]Br)([CH3:10])([CH3:9])[CH3:8].[H-].[H-].[H-].[H-].[Li+].[Al+3].[NH4+].[Cl-].OS(O)(=O)=O.O1CCC[CH2:27]1>C(O)C>[CH3:8][C:7]([CH3:10])([CH3:27])[CH:9]=[CH:2][CH:3]=[CH:4][CH:5]=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 1118Sulfuric AcidHCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 979834-Methoxy-but-3-en-1-yneHCID 21226445Aluminium lithium hydrideHCID 178418586HCID 178418586, 화합물

생성물 1

HCID 545330256,6-Dimethylhepta-2,4-dienal

실험 절차

Freshly distilled 4-methoxy-but-3-en-1-yne is added dropwise under cooling to a solution of t-butyl-magnesium bromide in absolute tetrahydrofuran and the mixture stirred for 45 minutes at room temperature. The reaction mixture is first mixed with 13.6 g of ethanol, then, under cooling and inert gas atmosphere, reacted with 5.9 g of LiAlH4 and stirred overnight at room temperature. It is then mixed with saturated aqueous NH4Cl under cooling, acidified with H2SO4 and extracted with ether. The pure product is obtained by vacuum distillation b.p. (bulb tube) 50°/0.26 mbar.

후처리

  1. temperatureunder cooling
  2. stirringstirred overnight at room temperature
  3. temperatureunder cooling
  4. extractionextracted with ether
  5. customThe pure product is obtained by vacuum distillation b.p
  6. custom(bulb tube) 50°/0.26 mbar

출처 및 근거

ORD 기록
ord-c5a68c4760de42b388f6b92b21bc938b
출처 데이터셋
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04382951

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시약·촉매·용매 1

HCID 702Ethanol용매