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Hydrochloric Acid → HCID 178509695, 화합물

HRID 431998
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HRID 431998 반응식
[C:1]([C:3]1[CH:4]=[C:5]([C:9]2[N:10]=[CH:11][N:12](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH:13]=2)[CH:6]=[CH:7][CH:8]=1)#[N:2].Cl>O1CCCC1>[C:1]([C:3]1[CH:4]=[C:5]([C:9]2[N:10]=[CH:11][NH:12][CH:13]=2)[CH:6]=[CH:7][CH:8]=1)#[N:2]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 219426904-(3-cyanophenyl)-1-trityl-1H-imidazole

생성물 1

HCID 178509695HCID 178509695, 화합물수율 72%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 4-(3-cyanophenyl)-1-trityl-1H-imidazole (0.07 g, 0.17 mmol) in tetrahydrofuran (1.36 mL) was treated with 2N hydrochloric acid (0.68 mL) and the resulting mixture was heated at reflux for 45 minutes. After cooling the reaction mixture was concentrated in vacuo and the residue dissolved in dichloromethane (20 mL). The organic phase was successively washed with 1N sodium hydroxide (10 mL), water (20 mL) and brine (20 mL). The organic solution was dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. Silica gel chromatography of the residues using 3% methanol in dichloromethane afforded 0.02 g (72%) of 4-(3-cyanophenyl)imidazole as a white solid.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for 45 minutes
  3. temperatureAfter cooling the reaction mixture
  4. concentrationwas concentrated in vacuo
  5. dissolutionthe residue dissolved in dichloromethane (20 mL)
  6. washThe organic phase was successively washed with 1N sodium hydroxide (10 mL), water (20 mL) and brine (20 mL)
  7. dry with materialThe organic solution was dried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5bf36b5f3bef435fa49030720762c082
출처 데이터셋
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06660753B2

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