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Sodium Azide → 6-Methoxyindan-1-ylmethylazide

HRID 1762574
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HRID 1762574 반응식
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8][CH:9]2[CH2:12]OS(C)(=O)=O)=[CH:5][CH:4]=1.[N-:18]=[N+:19]=[N-:20].[Na+]>CS(C)=O>[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8][CH:9]2[CH2:12][N:18]=[N+:19]=[N-:20])=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 17883324Methanesulphonic acid (6-methoxyindan-1-ylmethyl) ester

생성물 1

HCID 230442196-Methoxyindan-1-ylmethylazide

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

12.8 g (50 mmol) of methanesulphonic acid (6-methoxyindan-1-ylmethyl) ester and 5.2 g (80 mmol) of sodium azide are dissolved in 130 ml of dimethyl sulphoxide and stirred at 80° for 1 hour. The reaction mixture is poured onto ice-water and extracted by shaking with diethyl ether. The organic phases are washed twice with saturated sodium chloride solution, dried over magnesium sulphate and concentrated to dryness by evaporation under reduced pressure. 9.7 g of crude, oily 6-methoxyindan-1-ylmethylazide are obtained as residue.

후처리

  1. additionThe reaction mixture is poured onto ice-water
  2. extractionextracted
  3. stirringby shaking with diethyl ether
  4. washThe organic phases are washed twice with saturated sodium chloride solution
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated to dryness by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-310a4b1ec8814041abd90ec554d25036
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04833169

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