反応式
[NH4+].[Cl-].[NH:3]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([C:12]2[CH:17]=[CH:16][N:15]=[C:14]([NH:18][C:19]3[CH:24]=[C:23]([N+:25]([O-])=O)[C:22]([N:28]4[CH2:33][CH2:32][N:31]([CH3:34])[CH2:30][CH2:29]4)=[CH:21][C:20]=3[O:35][CH3:36])[N:13]=2)=[CH:4]1>O.C(O)C.[Fe]>[NH:3]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([C:12]2[CH:17]=[CH:16][N:15]=[C:14]([NH:18][C:19]3[CH:24]=[C:23]([NH2:25])[C:22]([N:28]4[CH2:33][CH2:32][N:31]([CH3:34])[CH2:30][CH2:29]4)=[CH:21][C:20]=3[O:35][CH3:36])[N:13]=2)=[CH:4]1参加物
6
反応物 2
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 105 °C
実験手順
A solution of NH4Cl (0.021 g, 0.38 mmol) in water (3 mL) was added in one portion to a stirred suspension of 4-(1H-indol-3-yl)-N-[2-methoxy-4-(4-methylpiperazin-1-yl)-5-nitrophenyl]pyrimidin-2-amine (Intermediate 67, 0.235 g, 0.51 mmol) and iron (0.171 g, 3.07 mmol) in ethanol (9 mL) and the mixture was stirred at 105° C. for 18 h. The mixture was then concentrated in vacuo and the resulting residue was dissolved in DMF (20 mL). Purification by ion exchange chromatography, using an SCX column, eluting with 0.35M methanolic ammonia in CH2Cl2 and concentration of the appropriate fractions gave the title compound (0.206 g, 94%) as a yellow solid; m/z: ES+ MH+ 430.51.
後処理
- concentrationThe mixture was then concentrated in vacuo
- dissolutionthe resulting residue was dissolved in DMF (20 mL)
- customPurification by ion exchange chromatography
- washeluting with 0.35M methanolic ammonia in CH2Cl2 and concentration of the appropriate fractions
出典と根拠
- ORDレコード
- ord-488bea28bb164e798bdab266afe93115
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08946235B2
関連ノート
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