Methylamine → 4-(2-Methylamino-pyrimidin-4-yloxy)-benzene-1,2-diamine

HRID 491646ノート

反応式

HRID 491646 の反応式
CS([C:5]1[N:10]=[C:9]([O:11][C:12]2[CH:13]=[C:14]([NH2:19])[C:15]([NH2:18])=[CH:16][CH:17]=2)[CH:8]=[CH:7][N:6]=1)(=O)=O.[CH3:20][NH2:21]>C1COCC1>[CH3:20][NH:21][C:5]1[N:10]=[C:9]([O:11][C:12]2[CH:13]=[C:14]([NH2:19])[C:15]([NH2:18])=[CH:16][CH:17]=2)[CH:8]=[CH:7][N:6]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 177564964-(2-Methanesulfonyl-pyrimidin-4-yloxy)-benzene-1,2-diamine

生成物 1

HCID 177554024-(2-Methylamino-pyrimidin-4-yloxy)-benzene-1,2-diamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
80 °C

実験手順

To a solution of 4-(2-methanesulfonyl-pyrimidin-4-yloxy)-benzene-1,2-diamine (Step B, 400 mg, 1.4 mmol, 1.0 eq) in anhydrous THF (4 mL) was added 1 mL of 2 M CH3NH2 in THF (2 mmol, 1.4 eq). The solution was heated to 80° C. for 1 h. The THF was removed under reduced pressure. The crude was purified by column chromatography (0-10% MeOH/CH2Cl2 with 1% NH4OH) to yield 4-(2-methylamino-pyrimidin-4-yloxy)-benzene-1,2-diamine.

後処理

  1. customThe THF was removed under reduced pressure
  2. customThe crude was purified by column chromatography (0-10% MeOH/CH2Cl2 with 1% NH4OH)

出典と根拠

ORDレコード
ord-e81dd832725f48158bdf355ccb60d16f
出典データセット
uspto-grants-2009_05
特許番号
US07531553B2

反応ノート

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