Potassium Carbonate → Ethyl 7-[methyl-[2-[(2,2,2-trifluoroacetyl)amino]ethyl]amino]heptanoate

HRID 1356453ノート

反応式

HRID 1356453 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]([NH:5][CH2:6][CH2:7][NH:8][CH3:9])=[O:4].Br[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:9][N:8]([CH2:7][CH2:6][NH:5][C:3](=[O:4])[C:2]([F:10])([F:11])[F:1])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 122490Ethyl 7-bromoheptanoateHCID 107022842,2,2-trifluoro-N-[2-(methylamino)ethyl]acetamide

生成物 1

HCID 18508347Ethyl 7-[methyl-[2-[(2,2,2-trifluoroacetyl)amino]ethyl]amino]heptanoate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2,2,2-trifluoro-N-[2-(methylamino)ethyl]acetamide (5 g) in DMF (50 ml) were added ethyl 7-bromoheptanoate (3.6 ml) and potassium carbonate (7.7 g) and stirring was continued at room temperature for 18 hr. Potassium carbonate was removed by filtration and saturated aqueous sodium bicarbonate and water was added to the filtrate, which was extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride sequentially, dried with sodium sulfate, and concentrated. The residue was dissolved in toluene and purified by passing through the silica gel column (eluent; hexane to hexane-ethyl acetate (4:1) to ethyl acetate) to obtain the titled compound as a crude material (7 g).

後処理

  1. customPotassium carbonate was removed by filtration and saturated aqueous sodium bicarbonate and water
  2. additionwas added to the filtrate, which
  3. extractionwas extracted with ethyl acetate
  4. washThe organic layer was washed with water and saturated aqueous sodium chloride sequentially
  5. dry with materialdried with sodium sulfate
  6. concentrationconcentrated
  7. dissolutionThe residue was dissolved in toluene
  8. custompurified

出典と根拠

ORDレコード
ord-5233f0b68a1c48e59968bcdd34eefbb1
出典データセット
uspto-grants-2003_07
特許番号
US06586475B1

反応ノート

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