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Potassium Carbonate → HCID 178501112、化合物

HRID 538054
ノート
印刷プレビュー

反応式

HRID 538054 の反応式
C([O-])([O-])=O.[K+].[K+].F[C:8]1[CH:13]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:10][C:9]=1[N+:18]([O-:20])=[O:19].[CH3:21][O:22][C:23]([C@H:25]1[CH2:30][CH2:29][C@H:28]([CH2:31][NH2:32])[CH2:27][CH2:26]1)=[O:24]>CN(C=O)C>[CH3:21][O:22][C:23]([C@H:25]1[CH2:30][CH2:29][C@H:28]([CH2:31][NH:32][C:8]2[CH:13]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:10][C:9]=2[N+:18]([O-:20])=[O:19])[CH2:27][CH2:26]1)=[O:24]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 37221693-fluoro-4-nitrobenzotrifluorideHCID 178501118HCID 178501118、化合物

生成物 1

HCID 178501112HCID 178501112、化合物収率 86.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

K2CO3 (1.6 g, 11.7 mmol), 2-Fluoro-1-nitro-4-trifluoromethyl-benzene (1.22 g, 5.8 mmol) and trans-4-Aminomethyl-cyclohexanecarboxylic acid methyl ester (1.00 g, 5.84 mmol) were dissolved in DMF (10 ml). The mixture was stirred at 50° C. overnight. The solvent was removed under reduced pressure and the crude product dissolved in DCM (15 ml) and washed with water (20 ml) and then with a solution of citric acid (1M, 5 ml). The organic solution was dried over Na2SO4, filtered and the solvent removed by evaporation to give solid material. This was washed with cyclohexane and then with isopropyl ether and purified by silica column using DCM/cyclo hexane (1:1) as eluent. 1.8 g (yield 86%) of the title compound were isolated.

後処理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe crude product dissolved in DCM (15 ml)
  3. washwashed with water (20 ml)
  4. dry with materialThe organic solution was dried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent removed by evaporation
  7. customto give solid material
  8. washThis was washed with cyclohexane
  9. customwith isopropyl ether and purified by silica column

出典と根拠

ORDレコード
ord-2d482fafe8e649b8841a8f7e5390fded
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08865704B2

反応ノート

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