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Water → HCID 22259358, 화합물

HRID 1610974
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HRID 1610974 반응식
C(=O)([O-])[O-].[K+].[K+].I[CH2:8][CH2:9][CH2:10][CH2:11][C:12]1[CH:36]=[CH:35][C:15]([O:16][CH2:17][C:18]2[N:19]=[C:20](/[CH:23]=[CH:24]/[C:25]3[CH:30]=[CH:29][C:28]([C:31]([F:34])([F:33])[F:32])=[CH:27][CH:26]=3)[O:21][CH:22]=2)=[CH:14][CH:13]=1.[NH:37]1[CH:41]=[C:40]([C:42]([O:44][CH2:45][CH3:46])=[O:43])[N:39]=[N:38]1.O>CN(C)C=O>[F:32][C:31]([F:34])([F:33])[C:28]1[CH:29]=[CH:30][C:25](/[CH:24]=[CH:23]/[C:20]2[O:21][CH:22]=[C:18]([CH2:17][O:16][C:15]3[CH:35]=[CH:36][C:12]([CH2:11][CH2:10][CH2:9][CH2:8][N:37]4[CH:41]=[C:40]([C:42]([O:44][CH2:45][CH3:46])=[O:43])[N:39]=[N:38]4)=[CH:13][CH:14]=3)[N:19]=2)=[CH:26][CH:27]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 22259303HCID 22259303, 화합물HCID 178469944HCID 178469944, 화합물

생성물 1

HCID 22259358HCID 22259358, 화합물수율 24.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

Potassium carbonate (2.4 g) was added to a solution of 4-[[4-(4-iodobutyl)phenoxy]methyl]-2-{(E)-2-[4-(trifluoromethyl)phenyl]ethenyl}-1,3-oxazole (7.5 g) and ethyl 1H-1,2,3-triazole-4-carboxylate (2.1 g) in dimethylformamide (100 ml), and the mixture was stirred at 70° C. for 5 hr. After the reaction was completed, the reaction mixture was combined with water and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent; ethyl acetate:hexane=3:1), and recrystallized from ethyl acetate-hexane to give the titled compound (1.85 g) as a colorless crystal powder.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (eluent; ethyl acetate:hexane=3:1)
  6. customrecrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-20277d56cb6945349e7c7029359bf3f3
출처 데이터셋
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06984653B2

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