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Potassium Carbonate → HCID 13362794, 화합물

HRID 365059
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HRID 365059 반응식
[C:1]([C:3]1[CH:16]=[CH:15][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1)#[N:2].Br[CH:18]([CH3:28])[C:19]([NH:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:20].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[C:22]1([NH:21][C:19](=[O:20])[CH:18]([O:14][C:11]2[CH:12]=[CH:13][C:8]([O:7][C:6]3[CH:15]=[CH:16][C:3]([C:1]#[N:2])=[CH:4][CH:5]=3)=[CH:9][CH:10]=2)[CH3:28])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 991132-Bromo-N-phenylpropionamideHCID 45227124-(4-Hydroxyphenoxy)benzonitrile

생성물 1

HCID 13362794HCID 13362794, 화합물수율 68.8%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To 30 ml of acetone were added 1.06 g of 4-(4-cyanophenoxy)-phenol, 0.99 g of α-bromopropionanilide and 0.83 g of anhydrous potassium carbonate, and the mixture wask subjected to reflux for 16 hours with stirring. After the reaction mixture was cooled and separated from inorganic salts through filtration, acetone was distilled away therefrom. The residue was purified through a column-chromatography [silica gel, developed with ethyl acetate/n-hexane=1/1(V/V)] to give 1.07 g of the title compound (yield 60%), which was recrystallized from a mixed solvent of benzene-n-hexane to afford a crystal of melting point 133°-134° C.

후처리

  1. temperatureto reflux for 16 hours
  2. temperatureAfter the reaction mixture was cooled
  3. customseparated from inorganic salts through filtration, acetone
  4. distillationwas distilled away
  5. customThe residue was purified through a column-chromatography [silica gel

출처 및 근거

ORD 기록
ord-69b212377b6e44eb8aa82304a4803d6a
출처 데이터셋
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04608081

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