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N,N-Dimethylaniline → HCID 58499548, 화합물

HRID 910272
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HRID 910272 반응식
[Al+3].[Cl-].[Cl-].[Cl-].C1(N(C)C)C=CC=CC=1.C([O:21][CH2:22][C@@H:23]([NH:39][S:40]([C:43]1[CH:48]=[CH:47][C:46]([Cl:49])=[C:45]([Cl:50])[CH:44]=1)(=[O:42])=[O:41])[C:24]1[N:28]([CH2:29][CH3:30])[C:27]([O:31][C:32]2[CH:37]=[CH:36][C:35]([F:38])=[CH:34][CH:33]=2)=[N:26][N:25]=1)C1C=CC=CC=1.CCOC(C)=O>C(Cl)Cl>[Cl:50][C:45]1[CH:44]=[C:43]([S:40]([NH:39][C@@H:23]([C:24]2[N:28]([CH2:29][CH3:30])[C:27]([O:31][C:32]3[CH:33]=[CH:34][C:35]([F:38])=[CH:36][CH:37]=3)=[N:26][N:25]=2)[CH2:22][OH:21])(=[O:41])=[O:42])[CH:48]=[CH:47][C:46]=1[Cl:49]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 949N,N-DimethylanilineHCID 8857Ethyl AcetateHCID 6451240Aluminum(III) ChlorideHCID 58499692HCID 58499692, 화합물

생성물 1

HCID 58499548HCID 58499548, 화합물수율 93.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

AlCl3 (49 mg) and PhNMe2 (148 mg) were added to a solution of the compound (69 mg) of Example 23 in CH2Cl2 (2.0 ml), and the mixture was stirred at room temperature for one hour. Then, AcOEt was added, and the mixture was washed with 1N hydrochloric acid and thereafter with saturated aqueous sodium chloride. The organic layer was dried (Na2SO4), filtered, and evaporated under reduced pressure to remove the solvent. Then, the resulting crude product was purified by column chromatography (OH SiO2, AcOEt/hexane=2/1) to give 54 mg of the titled compound (Compound 696) as a colorless powder.

후처리

  1. washthe mixture was washed with 1N hydrochloric acid
  2. dry with materialThe organic layer was dried (Na2SO4)
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. customto remove the solvent
  6. customThen, the resulting crude product was purified by column chromatography (OH SiO2, AcOEt/hexane=2/1)

출처 및 근거

ORD 기록
ord-f001a18793554eaf8b4320d3becd13d5
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022091B2

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