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

HRID 1061879

반응식

HRID 1061879 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d7a6da0d23cd412b8dd5363bbc21bb3f
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06960586B2

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