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Sodium Iodide → HCID 68433156, 화합물

HRID 1867410
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HRID 1867410 반응식
[Cl:1][C:2]1[CH:3]=[C:4](/[CH:9]=[CH:10]/[C:11]([N:13]2[CH2:19][CH2:18][C:17](=[O:20])[N:16]([CH2:21][CH2:22][CH2:23]OS(C)(=O)=O)[CH2:15][CH2:14]2)=[O:12])[CH:5]=[CH:6][C:7]=1[Cl:8].[I-:29].[Na+]>CC(=O)CC>[Cl:1][C:2]1[CH:3]=[C:4](/[CH:9]=[CH:10]/[C:11]([N:13]2[CH2:19][CH2:18][C:17](=[O:20])[N:16]([CH2:21][CH2:22][CH2:23][I:29])[CH2:15][CH2:14]2)=[O:12])[CH:5]=[CH:6][C:7]=1[Cl:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 5238Sodium IodideHCID 86615869HCID 86615869, 화합물

생성물 1

HCID 68433156HCID 68433156, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

반응 조건

온도
95 °C

실험 절차

A solution of 0.50 g (1.11 mmol) of crude methanesulfonic acid 3-{4-[(E)-3-(3,4-dichloro-phenyl)-acryloyl]-7-oxo-[1,4]diazepan-1-yl}-propyl ester in 20 ml of 2-butanone was treated with 0.33 g (2.23 mmol) of sodium iodide and stirred at 95° C. for 30 min. The reaction was cooled, evaporated, suspended in 60 ml dichloromethane/Et2O (1:3), filtered and the organic solvent discarded. The residue was then washed again with dichloromethane to give after evaporation 0.27 g (51%) of the title compound as white solid. MS: 481.0 (MH+, 2Cl).

후처리

  1. temperatureThe reaction was cooled
  2. customevaporated
  3. filtrationfiltered
  4. washThe residue was then washed again with dichloromethane
  5. customto give
  6. customafter evaporation 0.27 g (51%) of the title compound as white solid

출처 및 근거

ORD 기록
ord-e2f8e9b1f7d54d94b938978062295724
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07632829B2

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