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Sodium Bicarbonate → (2Z)-3-Amino-2-cyano-4-ethyl-2-hexene

HRID 2262448
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HRID 2262448 반응식
[NH2:1]/[C:2](/[CH:9]([CH2:12][CH3:13])[CH2:10][CH3:11])=[C:3](/[C:7]#[N:8])\[C:4](Cl)=O.C([O-])(O)=O.[Na+]>C(#N)C.O>[NH2:1]/[C:2](/[CH:9]([CH2:10][CH3:11])[CH2:12][CH3:13])=[C:3](\[C:7]#[N:8])/[CH3:4]
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참가 물질

5

반응물 2

HCID 516892Sodium BicarbonateHCID 86595835(2Z)-3-Amino-2-cyano-4-ethyl-2-hexenoyl chloride

생성물 1

HCID 86595836(2Z)-3-Amino-2-cyano-4-ethyl-2-hexene수율 87.6%

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

반응 조건

온도
25 °C

실험 절차

3 g (15 mmol) of (2Z)-3-amino-2-cyano-4-ethyl-2-hexenoyl chloride dissolved in acetonitrile were added dropwise to a solution of 2.6 g (30 mmol) NaHCO3 in water. The solution was stirred at 25° C. for 30 min, then concentrated to dryness and the residue was taken up in methanol. The precipitate was seperated and the filtrate concencentrated to dryness again. The residue was dissolved in water and saturated KHSO4-solution was added. Filtration of the precipitate gave 2 g of the title compound (73% of theory) as a colorless solid (m. p. 150° C.)

후처리

  1. concentrationconcentrated to dryness
  2. customThe precipitate was seperated
  3. dissolutionThe residue was dissolved in water
  4. additionsaturated KHSO4-solution was added
  5. filtrationFiltration of the precipitate

출처 및 근거

ORD 기록
ord-12016601758e4ca2949e51d73b61092e
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07851411B2

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