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Sodium Iodide → HCID 57037785, 화합물

HRID 2251952
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HRID 2251952 반응식
[CH:1]([N:14]([CH3:19])[CH2:15][CH2:16][NH:17][CH3:18])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[CH2:21][CH2:22][CH2:23][CH2:24][N:25]1[C:29](=[O:30])[C:28]2=[CH:31][CH:32]=[CH:33][CH:34]=[C:27]2[C:26]1=[O:35].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C=O)C>[CH:1]([N:14]([CH3:19])[CH2:15][CH2:16][N:17]([CH3:18])[CH2:21][CH2:22][CH2:23][CH2:24][N:25]1[C:29](=[O:30])[C:28]2[C:27](=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:26]1=[O:35])([C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 93575N-(4-Bromobutyl)phthalimideHCID 13984386N~1~-(Diphenylmethyl)-N~1~,N~2~-dimethylethane-1,2-diamine

생성물 1

HCID 57037785HCID 57037785, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

13.9 g (54,7 mmol) N1-benzhydryl-N1,N2-dimethyl-ethan-1,2-diamine, 15.4 g (54.7 mmol) N-(4-bromobutyl)-phthalimide, 15.1 g (109.5 mmol) potassium carbonate and 1.6 g (10.6 mmol) sodium iodide are stirred for four hours in DMF at 70° C. After cooling, the mixture is concentrated under vacuum and the residue is distributed between chloroform and water. The organic phase is dried over sodium sulfate and evaporated under vacuum until dry. The purification occurs by chromatography on silica gel with CHCl3/CH3OH (100/0 to 99/1): Yield 20.8 g (83%).

후처리

  1. temperatureAfter cooling
  2. concentrationthe mixture is concentrated under vacuum
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. customevaporated under vacuum
  5. customuntil dry
  6. customThe purification

출처 및 근거

ORD 기록
ord-2429388e86984313a4cc49e38965bebd
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07320993B1

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