Ethylamine → N-(2-Bromo-6-methoxy-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide

HRID 53532ノート

反応式

HRID 53532 の反応式
[Br:1][C:2]1[C:7]([NH:8][C:9]([C:11]2[C:12](Cl)=[N:13][CH:14]=[CH:15][CH:16]=2)=[O:10])=[C:6]([CH3:18])[CH:5]=[C:4]([O:19][CH3:20])[N:3]=1.O1CCOCC1.[CH2:27]([NH2:29])[CH3:28]>C(OCC)(=O)C>[Br:1][C:2]1[C:7]([NH:8][C:9]([C:11]2[C:12]([NH:29][CH2:27][CH3:28])=[N:13][CH:14]=[CH:15][CH:16]=2)=[O:10])=[C:6]([CH3:18])[CH:5]=[C:4]([O:19][CH3:20])[N:3]=1

参加物

5

反応物 3

HCID 6341EthylamineHCID 312751,4-DioxaneHCID 19960021N-(2-bromo-6-methoxy-4-methyl-3-pyridinyl)-2-chloro-3-pyridinecarboxamide

生成物 1

HCID 19960032N-(2-Bromo-6-methoxy-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide収率 44.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
140 °C

実験手順

A mixture of N-(2-bromo-6-methoxy-4-methyl-3-pyridinyl)-2-chloro-3-pyridinecarboxamide (2.1 g), dioxane (10 ml), and ethylamine (0.5 g) was heated to 140° C. in a sealed tube for 5 hours. The cooled mixture was diluted with ethyl acetate, washed with water, and the organic phase was dried (anhydrous magnesium sulfate) and concentrated. The product was purified on a silica gel column (methylene chloride/ethyl acetate, 99:1) and crystallized by trituration with diisopropyl ether to give 0.95 g of the title compound.

後処理

  1. washwashed with water
  2. dry with materialthe organic phase was dried (anhydrous magnesium sulfate)
  3. concentrationconcentrated
  4. customThe product was purified on a silica gel column (methylene chloride/ethyl acetate, 99:1)
  5. customcrystallized by trituration with diisopropyl ether

出典と根拠

ORDレコード
ord-0d2446fa61c7432eb532efde6150e60e
出典データセット
uspto-grants-1997_04
特許番号
US05620974

反応ノート

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