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Allyl bromide → HCID 20360231、化合物

HRID 2082668
ノート
印刷プレビュー

反応式

HRID 2082668 の反応式
[CH:1]12[CH2:15][CH:6]([C:7](=[O:14])[C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=31)[CH2:5][NH:4][CH2:3][CH2:2]2.C(=O)([O-])[O-].[Na+].[Na+].[CH2:22](Br)[CH:23]=[CH2:24]>C(O)C>[CH2:24]([N:4]1[CH2:3][CH2:2][CH:1]2[CH2:15][CH:6]([CH:7]([OH:14])[C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=32)[CH2:5]1)[CH:23]=[CH2:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7841Allyl bromideHCID 10340Sodium CarbonateHCID 20360238HCID 20360238、化合物

生成物 1

HCID 20360231HCID 20360231、化合物収率 74.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

20 ml of ethanol was added to 1 g of 2,3,4,5-tetrahydro-1,6-methano-1H-4-benzazonin-7(6H)-one and 0.63 g of sodium carbonate, and the mixture was heated and refluxed. Then, 0.72 g of allyl bromide was gradually added to the mixture, and the reaction mixture liquid was heated and refluxed for 5 hours. The mixture was cooled and filtered, and methanol and excessive allyl bromide were distilled from the filtrate. The residue was dissolved in 20 ml of methanol and cooled with ice water, and 0.15 g of sodium boron hydride was gradually added to the solution under agitation. Then, the mixture was agitated at room temperature for 2 hours. Methanol was distilled from the reaction mixture, and 15 ml of water was added to the residue and the mixture was shaken sufficiently. Then, the mixture was extracted with ether and the extract was subjected to distillation to remove ether therefrom. The residue was recrystallized from cyclohexane to obtain 0.9 g of 4-allyl-2,3,4,5,6,7-hexahydro-1,6-methano-1H-4 -benzazonin-7-ol in the form of a white crystal melting at 98° to 100° C.

後処理

  1. temperaturethe mixture was heated
  2. temperaturerefluxed
  3. temperaturethe reaction mixture liquid was heated
  4. temperaturerefluxed for 5 hours
  5. temperatureThe mixture was cooled
  6. filtrationfiltered
  7. distillationmethanol and excessive allyl bromide were distilled from the filtrate
  8. dissolutionThe residue was dissolved in 20 ml of methanol
  9. temperaturecooled with ice water, and 0.15 g of sodium boron hydride
  10. additionwas gradually added to the solution under agitation
  11. distillationMethanol was distilled from the reaction mixture, and 15 ml of water
  12. additionwas added to the residue
  13. stirringthe mixture was shaken sufficiently
  14. extractionThen, the mixture was extracted with ether
  15. distillationthe extract was subjected to distillation
  16. customto remove ether
  17. customThe residue was recrystallized from cyclohexane

出典と根拠

ORDレコード
ord-fc060b2c9d954c4f8710340c477f2fe6
出典データセット
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04082744

反応ノート

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