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

HRID 2262448
ノート
印刷プレビュー

反応式

HRID 2262448 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
25 °C

実験手順

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.)

後処理

  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

出典と根拠

ORDレコード
ord-12016601758e4ca2949e51d73b61092e
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07851411B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート