N,N-二甲基甲酰胺二甲基缩醛 → N'-[6-(2,6-dichlorophenyl)-2-{3-(diethylamino)propylamino}-pyrido[2,3-d]pyrimidin-7-yl]-N,N-dimethylformamidine

HRID 3450

反应方程式

HRID 3450 反应方程式
[NH2:1][C:2]1[C:3]([C:21]2[C:26]([Cl:27])=[CH:25][CH:24]=[CH:23][C:22]=2[Cl:28])=[CH:4][C:5]2[CH:10]=[N:9][C:8]([NH:11][CH2:12][CH2:13][CH2:14][N:15]([CH2:18][CH3:19])[CH2:16][CH3:17])=[N:7][C:6]=2[N:20]=1.[CH3:29][N:30]([CH:32](OC)OC)[CH3:31]>CN(C=O)C>[Cl:28][C:22]1[CH:23]=[CH:24][CH:25]=[C:26]([Cl:27])[C:21]=1[C:3]1[C:2]([N:1]=[CH:29][N:30]([CH3:32])[CH3:31])=[N:20][C:6]2[N:7]=[C:8]([NH:11][CH2:12][CH2:13][CH2:14][N:15]([CH2:18][CH3:19])[CH2:16][CH3:17])[N:9]=[CH:10][C:5]=2[CH:4]=1

参与物

4

反应物 2

HCID 78373N,N-二甲基甲酰胺二甲基缩醛HCID 53281146-(2,6-dichlorophenyl)-2-N-[3-(diethylamino)propyl]pyrido[2,3-d]pyrimidine-2,7-diamine

产物 1

HCID 5328174N'-[6-(2,6-dichlorophenyl)-2-{3-(diethylamino)propylamino}-pyrido[2,3-d]pyrimidin-7-yl]-N,N-dimethylformamidine收率 68%

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

To a suspension of 210 mg (1 mmol) of 7-amino-6-(2,6-dichlorophenyl)-2-[3-(diethylamino) propylamino]-pyrido[2,3-d]pyrimidine from Example 20 in 0.8 mL of DMF was added 0.8 mL of DMF dimethyl acetal. The mixture was stirred at room temperature for 5.5 hours, then concentrated in vacuo. The residual oil was distributed between dichloromethane and water. The organic phase was dried over magnesium sulfate, then concentrated to a glass that was crystallized from acetonitrile to give 160 mg (68%) of N'-[6-(2,6-dichlorophenyl)-2-{3-(diethylamino) propylamino}-pyrido[2,3-d]pyrimidin-7-yl]-N, N-dimethylformamidine, mp 100°-104° C.

后处理

  1. concentrationconcentrated in vacuo
  2. dry with materialThe organic phase was dried over magnesium sulfate
  3. concentrationconcentrated to a glass that
  4. customwas crystallized from acetonitrile

来源与证据

ORD记录
ord-3b18944e08c244489c0c882a36845a09
来源数据集
uspto-grants-1998_03
专利号
US05733913

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