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

HRID 637702ノート

反応式

HRID 637702 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 14798Sodium Hydroxide溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1a910469e55e4faaad73c7dd64de4c82
出典データセット
uspto-grants-1985_12
特許番号
US04558060

反応ノート

読み込み中…