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

HRID 8573
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인쇄 미리보기

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HRID 8573 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14797Potassium HydroxideHCID 160364063-Benzyl-7-(phenylsulfonyl)-9-oxa-3,7-diazabicyclo[3.3.1]nonaneHCID 21226445Aluminium lithium hydride

생성물 1

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

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-29a3d6e0dca643e485207c9d6fad4dea
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091198B1

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