反応式
Cl[C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][C:17]3[CH:22]=[CH:21][N:20]=[C:19]4[NH:23][CH:24]=[CH:25][C:18]=34)=[C:12]([F:26])[CH:11]=2)[CH:3]=1.C(N(C(C)C)C(C)C)C.[NH:36]1[CH2:41][CH2:40][O:39][CH2:38][CH2:37]1.CN(C=O)C>C(C(CCCC)CO)C>[F:26][C:12]1[CH:11]=[C:10]([NH:9][C:4]2[CH:3]=[C:2]([N:36]3[CH2:41][CH2:40][O:39][CH2:38][CH2:37]3)[N:7]=[C:6]([NH2:8])[N:5]=2)[CH:15]=[CH:14][C:13]=1[O:16][C:17]1[CH:22]=[CH:21][N:20]=[C:19]2[NH:23][CH:24]=[CH:25][C:18]=12参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 150 °C
実験手順
52 mg (0.14 mmol) of 6-chloro-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)-phenyl]pyrimidine-2,4-diamine (from example 60) are dissolved in 2.5 ml of 2-ethylhexanol. 0.24 ml of N-ethyldiisopropylamine and 36 mg (0.42 mmol) of morpholine are added, and the mixture is heated at 150° C. bath temperature for 20 hours. After cooling, a little DMF is added and the mixture is chromatographed on silica gel 60 (gradient column: mobile phase: DCM:methanol=50:1, then 3:1). This gives an oil which is purified by preparative HPLC.
後処理
- temperatureAfter cooling
- customthe mixture is chromatographed on silica gel 60 (gradient column
- customThis gives an oil which
- customis purified by preparative HPLC
出典と根拠
- ORDレコード
- ord-f27cdbac85644e37bba24b36a57db768
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737153B2
関連ノート
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