Hydrochloric Acid → HCID 178420123, 화합물

HRID 432002

반응식

HRID 432002 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[N:8]=[CH:9][N:10](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:11]=1.Cl>O1CCCC1>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[N:8]=[CH:9][NH:10][CH:11]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 219426882-(1-trityl-1H-imidazol-4-yl)pyridine

생성물 1

HCID 178420123HCID 178420123, 화합물수율 46.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of the crude 4-(2-pyridyl)-1-trityl-1H-imidazole (0.69g) in tetrahydrofuran (14 mL) was treated with 2 N hydrochloric acid (7.2 mL) and heated at reflux for 45 minutes. After cooling the reaction mixture was concentrated in vacuo and the residue was dissolved in dichloromethane (20 mL). The organic solution was successively washed with aqueous 1N sodium hydroxide (10 mL), water (20 mL) and brine (20 mL). The organic solution was then dried over anhydrous sodium sulfate, filtered, and concentrated in-vacuo to afford 0.12 g of crude 4-(2-pyridyl)imidazole, as a sticky white solid.

후처리

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

출처 및 근거

ORD 기록
ord-53d968e1a3174d4f8f50d9e6161031f7
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660753B2

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