Dimethylformamide → HCID 15953319, 화합물

HRID 271450노트

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HRID 271450 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[C:12]([NH:14][CH:15]([CH3:17])[CH3:16])[N:11]3[C:18](=[O:21])[NH:19][N:20]=[C:10]3[C:9]=2[C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=2)=[CH:4][CH:3]=1.[CH3:29]N(C=O)C.C(=O)([O-])[O-].[K+].[K+].CI>CCOC(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[C:12]([NH:14][CH:15]([CH3:17])[CH3:16])[N:11]3[C:18](=[O:21])[N:19]([CH3:29])[N:20]=[C:10]3[C:9]=2[C:22]2[CH:23]=[CH:24][C:25]([Cl:28])=[CH:26][CH:27]=2)=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 58772830HCID 58772830, 화합물

생성물 1

HCID 15953319HCID 15953319, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of crude 7,8-bis(4-chlorophenyl)-5-(isopropylamino)-[1,2,4]triazolo[4,3-c]pyrimidin-3(2H)-one, DMF (0.7 mL), and potassium carbonate (21 mg, 0.15 mmol) was added methyl iodide (213 mg, 1.5 mmol). The resulting reaction mixture was stirred at room temperature for 3 h. The reaction mixture was then diluted with EtOAc, washed with water and saturated aqueous NaCl, dried (Na2SO4), and concentrated at reduced pressure. The residue was purified by preparative reverse phase HPLC to obtain 14 mg (65% over two steps) of the title compound as a light yellow solid. HPLC/MS: retention time=4.54 min, [M+H]30 =428.

후처리

  1. customThe resulting reaction mixture
  2. washwashed with water and saturated aqueous NaCl
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated at reduced pressure
  5. customThe residue was purified by preparative reverse phase HPLC

출처 및 근거

ORD 기록
ord-af07555976654c5aaa7291cf8e7e2d67
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452892B2

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