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Sodium Iodide → 1,3-Dihydro-3-(3-iodopropyl)-7,8-dimethoxy-2H-3-benzazepin-2-one

HRID 487559
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HRID 487559 반응식
[CH3:1][O:2][C:3]1[C:18]([O:19][CH3:20])=[CH:17][C:6]2[CH2:7][C:8](=[O:16])[N:9]([CH2:12][CH2:13][CH2:14]Cl)[CH:10]=[CH:11][C:5]=2[CH:4]=1.[I-:21].[Na+]>CC(C)=O>[CH3:1][O:2][C:3]1[C:18]([O:19][CH3:20])=[CH:17][C:6]2[CH2:7][C:8](=[O:16])[N:9]([CH2:12][CH2:13][CH2:14][I:21])[CH:10]=[CH:11][C:5]=2[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 5238Sodium IodideHCID 130925033-(3-Chloropropyl)-1,3-dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one

생성물 1

HCID 190921901,3-Dihydro-3-(3-iodopropyl)-7,8-dimethoxy-2H-3-benzazepin-2-one수율 99%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A suspension of 12 g of 7,8-dimethoxy-3-[3-chloropropyl]-1,3-dihydro-2H-3-benzazepin-2-one obtained in accordance with the method described in the literature (Reiffer M. et al., J. Med. Chem. 1990; vol 33 (5): 1496-1504) and 6.2 g of sodium iodide in 50 cm3 of acetone are refluxed for 24 hours. After filtration and evaporation to dryness of the solvent, the residue is taken up in water and extracted with dichloromethane. The extract is separated off, dried over anhydrous magnesium sulphate and then concentrated in vacuo to yield 15.2 g of the desired compound.

후처리

  1. customobtained in accordance with the method
  2. temperatureare refluxed for 24 hours
  3. filtrationAfter filtration and evaporation to dryness of the solvent
  4. extractionextracted with dichloromethane
  5. customThe extract is separated off
  6. dry with materialdried over anhydrous magnesium sulphate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-4701aedfd940499fa1ac32e91c2faba0
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05296482

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