1-(2-Methoxyphenyl)piperazine → 6-(2-[4-(2-Methoxyphenyl)-piperazin-1-yl]-ethyl)-benzoxazolinone

HRID 637702노트

반응식

HRID 637702 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.Br[CH2:16][CH2:17][C:18]1[CH:27]=[CH:26][C:21]2[NH:22][C:23](=[O:25])[O:24][C:20]=2[CH:19]=1>O1CCOCC1.[OH-].[Na+]>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:16][CH2:17][C:18]2[CH:27]=[CH:26][C:21]3[NH:22][C:23](=[O:25])[O:24][C:20]=3[CH:19]=2)[CH2:11][CH2:10]1

참가 물질

5

반응물 2

HCID 13461-(2-Methoxyphenyl)piperazineHCID 133060876-Bromoethylbenzoxazolone

생성물 1

HCID 133435266-(2-[4-(2-Methoxyphenyl)-piperazin-1-yl]-ethyl)-benzoxazolinone수율 66.5%

시약·촉매·용매 2

HCID 14798Sodium Hydroxide용매HCID 312751,4-Dioxane용매

실험 절차

0.025 mol (4.82 g) of 1-(2-methoxyphenyl)-piperazine and 0.02 mol (4.85 g) of 6-(2-bromoethyl)-benzoxazolinone, dissolved beforehand in 50 cm3 of dioxane, were introduced into a 100 cm3 flask with a ground glass neck, fitted with a reflux condenser, and the mixture was then heated under reflux for 72 hours, with stirring. After cooling, filtration and drying, the precipitate formed was dissolved in a sufficient amount of a 3% aqueous solution of sodium hydroxide. A stream of carbon dioxide was then bubbled and the precipitate was filtered off, washed and dried. Recrystallisation from toluene gave 4.7 g of the title product having a melting point of 182°-184° C.

후처리

  1. additionwere introduced into a 100 cm3 flask with a ground glass neck
  2. customfitted with a reflux condenser
  3. temperaturethe mixture was then heated
  4. temperatureunder reflux for 72 hours
  5. temperatureAfter cooling
  6. filtrationfiltration
  7. customdrying
  8. customthe precipitate formed
  9. customA stream of carbon dioxide was then bubbled
  10. filtrationthe precipitate was filtered off
  11. washwashed
  12. customdried
  13. customRecrystallisation from toluene

출처 및 근거

ORD 기록
ord-1a910469e55e4faaad73c7dd64de4c82
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04558060

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