Methanol → N-benzyl-2-chloropyrimidin-4-amine
反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.[CH2:9]([NH2:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.CCN(C(C)C)C(C)C.CO>C1COCC1.C(Cl)Cl>[CH2:9]([NH:16][C:6]1[CH:5]=[CH:4][N:3]=[C:2]([Cl:1])[N:7]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1参加物
7
実験手順
To a solution of 2,4-dichloropyrimidine (0.15 g, 1.0 mmol), benzylamine (0.109 ml, 1.0 mmol) in THF was added DIPEA (0.526ml, 3.0 mmol) and the reaction was heated at reflux for 2 hours resulting in formation of a 4:1 mixture of regioisomers (desired versus undesired) by TLC (5% Methanol:methylene chloride). The reaction was stripped down in vacuo and purified by silica column (eluent: 2% methanol:methylene chloride) giving 0.12 g (0.548 mmol) of desired product 10 in 54% yield. LC/MS (M+1)=220
後処理
- temperaturethe reaction was heated
- temperatureat reflux for 2 hours
- custompurified by silica column (eluent: 2% methanol:methylene chloride)
出典と根拠
- ORDレコード
- ord-5a64242dda0e4caab75ae18cca28fc01
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08987454B2
反応ノート
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