Potassium Phosphate, Tribasic → 1-(6-Chloro-2-methylpyrimidin-4-yl)-3-(4-cyclopropylpyridin-3-yl)imidazolidin-2-one

HRID 523534

반응식

HRID 523534 반응식
[CH:1]1([C:4]2[CH:9]=[CH:8][N:7]=[CH:6][C:5]=2[N:10]2[CH2:14][CH2:13][NH:12][C:11]2=[O:15])[CH2:3][CH2:2]1.[Cl:16][C:17]1[CH:22]=[C:21](Cl)[N:20]=[C:19]([CH3:24])[N:18]=1.CN[C@@H]1CCCC[C@H]1NC.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>[Cu](I)I.O1CCOCC1>[Cl:16][C:17]1[N:18]=[C:19]([CH3:24])[N:20]=[C:21]([N:12]2[CH2:13][CH2:14][N:10]([C:5]3[CH:6]=[N:7][CH:8]=[CH:9][C:4]=3[CH:1]3[CH2:3][CH2:2]3)[C:11]2=[O:15])[CH:22]=1

참가 물질

7

반응물 4

HCID 62657Potassium Phosphate, TribasicHCID 2349974,6-Dichloro-2-methylpyrimidineHCID 2733821trans-N,N'-dimethyl-1,2-cyclohexanediamineHCID 709820071-(4-Cyclopropylpyridin-3-yl)imidazolidin-2-one

생성물 1

HCID 665764871-(6-Chloro-2-methylpyrimidin-4-yl)-3-(4-cyclopropylpyridin-3-yl)imidazolidin-2-one수율 15.4%

시약·촉매·용매 2

HCID 83717Copper iodide촉매HCID 312751,4-Dioxane용매

실험 절차

Using analogous reagents and reaction conditions as described in Example 1 above, 1-(4-cyclopropylpyridin-3-yl)imidazolidin-2-one (I-1d: 100 mg, 0.492 mmol) was reacted with 4,6-dichloro-2-methylpyrimidine (80.2 mg, 0.492 mmol), 1,4-dioxane (5 mL), copper iodide (9.3 mg, 0.049 mmol), trans-N,N′-dimethylcyclohexane-1,2-diamine (6.9 mg, 0.049 mmol) and potassium phosphate (313 mg, 1.47 mmol) to afford the crude product. Purification by column chromatography on silica gel (1% methanol in CHCl3) afforded 25 mg of the product (15% yield).

후처리

  1. customreagents and reaction conditions
  2. customto afford the crude product
  3. customPurification by column chromatography on silica gel (1% methanol in CHCl3)

출처 및 근거

ORD 기록
ord-dd7f4bf40bbd492481757a53a8a37875
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09339501B2

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