Acetonitrile → HCID 69671093、化合物

HRID 529876ノート

反応式

HRID 529876 の反応式
Cl[C:2]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[Cl:12])=[CH:3][C:4]#[N:5].Cl.[CH2:14]([CH:16]1[CH2:18][CH:17]1[NH2:19])C.[CH3:20]C#N>>[Cl:12][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[C:2]([NH:19][CH:17]([CH:16]([CH3:14])[CH3:18])[CH3:20])=[CH:3][C:4]#[N:5]

参加物

4

反応物 3

HCID 6342AcetonitrileHCID 129536982-Ethylcyclopropan-1-amine hydrochlorideHCID 713346313-Chloro-3-(2-chlorophenyl)prop-2-enenitrile

生成物 1

HCID 69671093HCID 69671093、化合物収率 89%

実験手順

To a solution of 3-chloro-3-(2-chlorophenyl)acrylonitrile (1.2 g, 6.05 mmol, 1 eq.) in 15 ml of MeCN was added 2-ethylcyclopropanamine hydrochloride (0.633 g, 7.27 mmol, 1.2 eq.) followed by TEA (0.919 g, 7.08 mmol, 1.5 eq.). The reaction was microwaved (130° C., 2000 s, fixed hold, high absorption) and the solvent evaporated. The residual oil was triturated in ethyl acetate and the white solid removed by filtration. After concentration under vacuum, the residual oil was subjected to column chromatography to give 3-(2-chlorophenyl)-3-[(3-methylbutan-2-yl)amino]acrylonitrile (1.36 g, 89% yield).

後処理

  1. customThe reaction was microwaved
  2. custom(130° C., 2000 s, fixed hold, high absorption)
  3. customthe solvent evaporated
  4. customThe residual oil was triturated in ethyl acetate
  5. customthe white solid removed by filtration
  6. concentrationAfter concentration under vacuum

出典と根拠

ORDレコード
ord-b66505aed2234931a4c81b0e636f7142
出典データセット
uspto-grants-2016_05
特許番号
US09351489B2

反応ノート

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