Acetic Acid → 2-({[(4-Fluorophenyl)(phenyl)methyl]amino}methylidene)butanedinitrile

HRID 730423노트

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HRID 730423 반응식
[K].[CH:2]([CH:4]([CH2:7][C:8]#[N:9])[C:5]#[N:6])=O.[F:10][C:11]1[CH:16]=[CH:15][C:14]([CH:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[NH2:18])=[CH:13][CH:12]=1.C(O)(=O)C>O>[F:10][C:11]1[CH:12]=[CH:13][C:14]([CH:17]([NH:18][CH:2]=[C:4]([CH2:7][C:8]#[N:9])[C:5]#[N:6])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:15][CH:16]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 111832724-Fluoro-α-phenylbenzenemethanamineHCID 86606793HCID 86606793, 화합물

생성물 1

HCID 690558642-({[(4-Fluorophenyl)(phenyl)methyl]amino}methylidene)butanedinitrile

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

To a solution of formyl succinonitrile potassium salt (7.26 g, 49.7 mmol) and 1-(4-fluorophenyl)-1-phenylmethaneamine (11.0 g, 54.7 mmol) in water-(20 ml) was added acetic acid (20 ml) at room temperature, the mixture was stirred at 100° C. for 30 minutes, and the solvent was distilled off under reduced pressure. The residue was poured into iced water, made basic by adding potassium carbonate and then extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to give the objective product as a solid material.

후처리

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionThe residue was poured into iced water
  3. additionby adding potassium carbonate
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-3fbc576e9c1547baab609e75c9ee59f5
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582651B2

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