反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:10]3[CH2:18][NH:17][CH2:16][CH2:15][C:11]=3[N:12]=[CH:13][N:14]=2)=[CH:4][CH:3]=1.Cl[C:20]1[C:25]([Cl:26])=[CH:24][CH:23]=[CH:22][N:21]=1.C(N(CC)C(C)C)(C)C>O1CCOCC1.CN(C)C(=O)C>[Cl:26][C:25]1[C:20]([N:17]2[CH2:16][CH2:15][C:11]3[N:12]=[CH:13][N:14]=[C:9]([NH:8][C:5]4[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=4)[C:10]=3[CH2:18]2)=[N:21][CH:22]=[CH:23][CH:24]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 150 °C
実験手順
N-(4-Fluorophenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (0.47 g, 1.92 mmol) was dissolved in a mixture of dioxane/N,N-dimethylacetamide (4:1) (3 mL). To the mixture was added 2,3-dichloropyridine (420 mg, 2.86 mmol) and N,N-diisopropylethylamine (0.38 mL, 2.2 mmol). The mixture was heated at 150° C. in a Personal Chemistry microwave for 16 h. The solvents were removed under vacuum and the residue was dissolved in ethyl acetate and washed with sat. NaHCO3 and brine. The organic layer was dried over Na2SO4, filtered and evaporated to give a brown residue. The residue was purified by silica gel chromatography using a gradient of ethyl acetate:hexane (0-100%) to give the desired compound as an off-white powder (200 mg, 30%).
後処理
- customThe solvents were removed under vacuum
- dissolutionthe residue was dissolved in ethyl acetate
- washwashed with sat. NaHCO3 and brine
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- customevaporated
- customto give a brown residue
- customThe residue was purified by silica gel chromatography
出典と根拠
- ORDレコード
- ord-60bf7b0411ce46dcb33b6cf568ecec10
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745451B2
関連ノート
読み込み中…