Methylamine → 2,6-Dichloro-N-methylpyridin-4-amine

HRID 2387699ノート

反応式

HRID 2387699 の反応式
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[CH:5]=[C:4]([Cl:9])[N:3]=1.[CH3:10][NH2:11]>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([NH:11][CH3:10])[CH:5]=[C:4]([Cl:9])[N:3]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 27665Pyridine, 2,4,6-trichloro-

生成物 1

HCID 199573942,6-Dichloro-N-methylpyridin-4-amine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
22.5 °C

実験手順

2,4,6-Trichloropyridine (1800 g, 9.89 mol) was dissolved in ethanol (1800 mL). Methylamine 40% solution in ethanol (6.3 L) was added over 1 h and 40 min maintaining the reaction temperature between 20-25° C. The reaction was stirred for 14 hours at room temperature and concentrated. The product was filtered, washed with methyl t-butyl ether (1,500 ml) and dried to yield A1.6 (1200 g, 68%)

後処理

  1. concentrationconcentrated
  2. filtrationThe product was filtered
  3. washwashed with methyl t-butyl ether (1,500 ml)
  4. customdried
  5. customto yield A1.6 (1200 g, 68%)

出典と根拠

ORDレコード
ord-e2de492a0a8c4faba44875ca7c4f4792
出典データセット
uspto-grants-2012_09
特許番号
US08268855B2

反応ノート

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