1-Methylpiperazine → HCID 58446993、化合物

HRID 1045766ノート

反応式

HRID 1045766 の反応式
[Br:1][C:2]1[C:3]([NH2:12])=[C:4]([N+:9]([O-:11])=[O:10])[C:5](Cl)=[N:6][CH:7]=1.[CH3:13][N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1>C(O)C>[Br:1][C:2]1[C:3]([NH2:12])=[C:4]([N+:9]([O-:11])=[O:10])[C:5]([N:17]2[CH2:18][CH2:19][N:14]([CH3:13])[CH2:15][CH2:16]2)=[N:6][CH:7]=1

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 573366665-Bromo-2-chloro-3-nitropyridin-4-amine

生成物 1

HCID 58446993HCID 58446993、化合物収率 64.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
130 °C

実験手順

A 20 mL microwave reaction tube was charged with 5-bromo-2-chloro-3-nitropyridin-4-amine (1.0 g, 3.9 mmol), N-methylpiperazine (0.78 g, 7.8 mmol) and anhydrous ethanol (15 mL). The resulting solution was heated at 130° C. for 1 h in a Biotage microwave reactor. The solvent was evaporated and the residue was purified by flash column chromatography on silica gel with 10% MeOH in CH2Cl2, to afford 0.80 g (64%) of the product as a white solid. MS m/z: 316 (M+H+).

後処理

  1. customThe solvent was evaporated
  2. customthe residue was purified by flash column chromatography on silica gel with 10% MeOH in CH2Cl2

出典と根拠

ORDレコード
ord-ef7d6d8a11e84cbc848ee6f78e6caafa
出典データセット
uspto-grants-2013_10
特許番号
US08569300B2

反応ノート

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