Ethanol → 1-Propene-1,1,3-tricarbonitrile, 2-phenyl-

HRID 257717노트

반응식

HRID 257717 반응식
[C:1]([CH2:9][C:10]#[N:11])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:12](#[N:16])[CH2:13][C:14]#[N:15].C([O-])(=O)C.[NH4+].C(O)C>O.Cl>[C:2]1([C:1]([CH2:9][C:10]#[N:11])=[C:13]([C:12]#[N:16])[C:14]#[N:15])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 702EthanolHCID 8010MalononitrileHCID 64799BenzoylacetonitrileHCID 517165Ammonium Acetate

생성물 1

HCID 46214401-Propene-1,1,3-tricarbonitrile, 2-phenyl-

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매

실험 절차

A mixture of benzoylacetonitrile (9.94 g, 0.0685 mole), malononitrile (11.3 g, 0.17 mole), ammonium acetate (5.4 g, 0.07 mole) and ethanol (100 mL) was heated at reflux for 1.5 hours. After cooling to room temperature, the reaction mixture was diluted with water (50 mL) and concentrated hydrochloric acid (7.5 mL) was added dropwise over 5 minutes. The resulting precipitate was collected by filtration and washed with water and ligroin. The yield was 10.0 g (76%), m.p. 92°-98° C.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 1.5 hours
  3. additionwas added dropwise over 5 minutes
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with water and ligroin

출처 및 근거

ORD 기록
ord-88a687fee7d1467c8682d480baad5d94
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05264320

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