Sodium Trifluoroacetate → 5-Trifluoromethyl-2-(di-n-propylamino)indan

HRID 725926ノート

反応式

HRID 725926 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[CH2:7][CH:6]([N:11]([CH2:15][CH2:16][CH3:17])[CH2:12][CH2:13][CH3:14])[CH2:5]2.[F:18][C:19]([F:24])([F:23])C([O-])=O.[Na+]>CN1C=CC=CC1=O.C(OCC)(=O)C.[Cu]I>[F:18][C:19]([F:24])([F:23])[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[CH2:7][CH:6]([N:11]([CH2:15][CH2:16][CH3:17])[CH2:12][CH2:13][CH3:14])[CH2:5]2

参加物

6

反応物 2

HCID 517019Sodium TrifluoroacetateHCID 21221814(6-Bromo-indan-2-yl)-dipropyl-amine

生成物 1

HCID 197102305-Trifluoromethyl-2-(di-n-propylamino)indan

試薬・触媒・溶媒 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 8857Ethyl Acetate溶媒HCID 127551-Methyl-2(1H)-pyridinone溶媒

実験手順

A solution of 5-bromo-2-(di-n-propylamino)indan (Example 11), sodium trifluoroacetate, and copper (I) iodide in N-methylpyridone is heated at 160° C. for 4 h under nitrogen (Chem Lett 1981, 1719). The reaction mixture is cooled to room temperature and diluted with ethyl acetate. The mixture is filtered through a layer of Celite pad and the filtrate is washed with water, brine, dried (MgSO4), filtered, and concentrated. The oil is purified by liquid chromatography to give the title compound as a yellow oil.

後処理

  1. filtrationThe mixture is filtered through a layer of Celite pad
  2. washthe filtrate is washed with water, brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe oil is purified by liquid chromatography

出典と根拠

ORDレコード
ord-99091c0fa8264508863a54a7df4c6f40
出典データセット
uspto-grants-1998_01
特許番号
US05708018

反応ノート

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