N,N'-Dimethylethylenediamine → HCID 89691128, 화합물

HRID 2202878노트

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HRID 2202878 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][O:7][C:8]2[CH:13]=[CH:12][NH:11][C:10](=[O:14])[CH:9]=2)=[CH:4][CH:3]=1.Br[C:18]1[CH:19]=[CH:20][C:21]2[N:25]=[C:24]([CH2:26][CH:27]([CH3:29])[CH3:28])[N:23]([CH3:30])[C:22]=2[CH:31]=1.C(=O)([O-])[O-].[K+].[K+].CNCCNC>[Cu](I)I.O.CS(C)=O>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][O:7][C:8]2[CH:13]=[CH:12][N:11]([C:18]3[CH:19]=[CH:20][C:21]4[N:25]=[C:24]([CH2:26][CH:27]([CH3:28])[CH3:29])[N:23]([CH3:30])[C:22]=4[CH:31]=3)[C:10](=[O:14])[CH:9]=2)=[CH:4][CH:3]=1

참가 물질

8

반응물 4

HCID 8070N,N'-DimethylethylenediamineHCID 11430Potassium CarbonateHCID 21504713HCID 21504713, 화합물HCID 574978644-[(4-Chlorophenyl)methoxy]pyridin-2(1H)-one

생성물 1

HCID 89691128HCID 89691128, 화합물수율 11.2%

시약·촉매·용매 3

HCID 83717Copper iodide촉매HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

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온도
120 °C

실험 절차

A mixture of 4-((4-chlorobenzyl)oxy)pyridin-2(1H)-one (115 mg), 6-bromo-2-isobutyl-1-methyl-1H-benzimidazole (130 mg), potassium carbonate (202 mg), copper iodide (93 mg), N,N′-dimethylethylenediamine (0.052 ml) and DMSO (3 ml) was heated at 120° C. for 3 h under microwave irradiation. The mixture was poured into water and extracted with EtOAc. The organic layer was separated, washed with water and brine, dried over MgSO4 and concentrated in vacuo. The precipitate was collected by filtration, and washed with IPE and EtOAc to give the title compound (23 mg) as an off-white solid.

후처리

  1. extractionextracted with EtOAc
  2. customThe organic layer was separated
  3. washwashed with water and brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with IPE and EtOAc

출처 및 근거

ORD 기록
ord-6c853bbad04446e7a0d3827932cc1f9c
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09365540B2

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