Dimethylformamide dimethyl acetal → N'-[6-(2,6-dichlorophenyl)-2-{3-(diethylamino)propylamino}-pyrido[2,3-d]pyrimidin-7-yl]-N,N-dimethylformamidine

HRID 617962

反応式

HRID 617962 の反応式
[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

参加物

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 53281146-(2,6-dichlorophenyl)-2-N-[3-(diethylamino)propyl]pyrido[2,3-d]pyrimidine-2,7-diamine

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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. CIMS (1% ammonia in methane): m/z (relative intensity) 476 (MH+ +2, 60), 474 (MH+, 94), 361 (100).

後処理

  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

出典と根拠

ORDレコード
ord-1e99aca4fe1c41ed8f39c56b79d6e855
出典データセット
uspto-grants-1999_09
特許番号
US05952342

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