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Water → 3-Benzyl-9-oxa-3,7-diazabicyclo[3.3.1]nonane

HRID 8573
ノート
印刷プレビュー

反応式

HRID 8573 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH2:21][CH:20]2[O:22][CH:16]([CH2:17][N:18](S(C3C=CC=CC=3)(=O)=O)[CH2:19]2)[CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.[OH-].[K+]>O1CCCC1>[CH2:7]([N:14]1[CH2:21][CH:20]2[O:22][CH:16]([CH2:17][NH:18][CH2:19]2)[CH2:15]1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 14797Potassium HydroxideHCID 160364063-Benzyl-7-(phenylsulfonyl)-9-oxa-3,7-diazabicyclo[3.3.1]nonaneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 160364073-Benzyl-9-oxa-3,7-diazabicyclo[3.3.1]nonane

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

10.00 g (0.25 mol) of lithium aluminum hydride are introduced into 300 ml of absolute tetrahydrofuran and heated to reflux, and 18.00 g (50 mmol) of 7-benzyl-3-phenylsulfonyl-9-oxa-3,7-diazabicyclo[3.3.1]nonane, dissolved in 150 ml of absolute tetrahydrofuran, are added dropwise. The mixture is boiled under reflux for 48 hours, 10 ml portions of water, 15% strength potassium hydroxide solution and again water are added dropwise, and the organic salts are filtered off with suction and extracted by boiling twice with tetrahydrofuran. The tetrahydrofuran solutions are concentrated, and the residue is distilled under high vacuum. 5.30 g (43.5% of theory) of the product are obtained

後処理

  1. temperatureheated
  2. temperatureto reflux
  3. additionare added dropwise
  4. temperatureunder reflux for 48 hours
  5. filtrationthe organic salts are filtered off with suction
  6. extractionextracted
  7. concentrationThe tetrahydrofuran solutions are concentrated
  8. distillationthe residue is distilled under high vacuum
  9. custom5.30 g (43.5% of theory) of the product are obtained

出典と根拠

ORDレコード
ord-29a3d6e0dca643e485207c9d6fad4dea
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07091198B1

反応ノート

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