Acetonitrile → HCID 69671093, 화합물

HRID 529876노트

반응식

HRID 529876 반응식
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]

참가 물질

4

반응물 3

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

생성물 1

HCID 69671093HCID 69671093, 화합물수율 89%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b66505aed2234931a4c81b0e636f7142
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09351489B2

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