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Ammonia → HCID 21812866, 화합물

HRID 469762
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HRID 469762 반응식
[CH3:1][C:2]([CH3:9])([CH3:8])[C:3](=O)[CH2:4][C:5]#[N:6].[N+:10]([O-])([O-])=O.[NH4+].N>C(O)C>[NH2:10]/[C:3](/[C:2]([CH3:9])([CH3:8])[CH3:1])=[CH:4]\[C:5]#[N:6]
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참가 물질

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반응물 3

HCID 222AmmoniaHCID 22985Ammonium nitrateHCID 108871Pentanenitrile, 4,4-dimethyl-3-oxo-

생성물 1

HCID 21812866HCID 21812866, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 4,4-dimethyl-3-oxo-pentanenitrile (22 g, 175.76 mmol) in 250 mL of ethanol is added ammonium nitrate (21 g; 263.64 mmol). The mixture is stirred under reflux overnight while ammonia gas is bubbled through the solution. The mixture is cooled to room temperature and diluted with 100 mL of water. The mixture is concentrated under reduced pressure to remove most of the ethanol. Aqueous sodium hydroxide (140 mL, 0.3N) is added and the mixture is extracted with ether (2×200 mL). The combined organic layers are washed with 50 mL of water, dried over sodium sulfate, filtered and concentrated under reduced pressure to afford title compound. Assumed quantitative yield and used crude in subsequent reaction. ESI m/z 125=MH+

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후처리

  1. customis bubbled through the solution
  2. additiondiluted with 100 mL of water
  3. concentrationThe mixture is concentrated under reduced pressure
  4. customto remove most of the ethanol
  5. additionAqueous sodium hydroxide (140 mL, 0.3N) is added
  6. extractionthe mixture is extracted with ether (2×200 mL)
  7. washThe combined organic layers are washed with 50 mL of water
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9b401d22cc864c1393346885c03ca814
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08629157B2

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