Diisopropylamine → 6-bromo-N,N-diisopropyl-2-naphthamide

HRID 1061879

反応式

HRID 1061879 の反応式
[CH:1]([NH:4][CH:5]([CH3:7])[CH3:6])([CH3:3])[CH3:2].C(N(CC)CC)C.[Br:15][C:16]1[CH:17]=[C:18]2[C:23](=[CH:24][CH:25]=1)[CH:22]=[C:21]([C:26](Cl)=[O:27])[CH:20]=[CH:19]2>C1COCC1>[Br:15][C:16]1[CH:17]=[C:18]2[C:23](=[CH:24][CH:25]=1)[CH:22]=[C:21]([C:26]([N:4]([CH:5]([CH3:7])[CH3:6])[CH:1]([CH3:3])[CH3:2])=[O:27])[CH:20]=[CH:19]2

参加物

5

反応物 3

HCID 7912DiisopropylamineHCID 8471TriethylamineHCID 218796066-Bromo-2-naphthoyl chloride

生成物 1

HCID 218796396-bromo-N,N-diisopropyl-2-naphthamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution (800 mL) of diisopropylamine (112 mL) and triethylamine (112 mL) in THF was added dropwise a solution (400 mL) of 6-bromo-2-naphthoyl chloride in THF under ice-cooling. The mixture was stirred at room temperature for 1 hr. A half amount of the solvent was evaporated under reduced pressure, and the residue was diluted with ethyl acetate, washed successively with water, 1N aqueous sodium hydroxide solution, water and saturated brine and dried over magnesium sulfate. The solvent was evaporated and the obtained solid was washed with isopropyl ether to give the title compound (117 g) as colorless flakes.

後処理

  1. temperaturecooling
  2. customA half amount of the solvent was evaporated under reduced pressure
  3. additionthe residue was diluted with ethyl acetate
  4. washwashed successively with water, 1N aqueous sodium hydroxide solution, water and saturated brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated
  7. washthe obtained solid was washed with isopropyl ether

出典と根拠

ORDレコード
ord-d7a6da0d23cd412b8dd5363bbc21bb3f
出典データセット
uspto-grants-2005_11
特許番号
US06960586B2

関連ノート

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