Potassium Carbonate → HCID 21938673、化合物

HRID 1242251ノート

反応式

HRID 1242251 の反応式
I[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1.[Cl:9][C:10]1[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[C:11]=1[NH2:12].C(=O)([O-])[O-].[K+].[K+]>C1(C)C(C)=CC=CC=1.CCCCCCC.[Cu]>[Cl:9][C:10]1[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[C:11]=1[NH:12][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 122074-IodotolueneHCID 27340832-Chloro-4,6-difluoroaniline

生成物 1

HCID 21938673HCID 21938673、化合物

試薬・触媒・溶媒 3

HCID 23978Copper触媒HCID 7237O-Xylene溶媒HCID 8900Heptane溶媒

実験手順

A mixture of 4-iodotoluene (210 g, 0.96 mol), 2-chloro-4,6-difluoroaniline (204 g, 1.25 mol), copper powder (36 g, 0.57 mol), cuprous iodide (130 g, 0.68 mol), and potassium carbonate (118 g, 0.86 mol) in 500 ml of xylene is stirred vigorously and heated to reflux in a flask fitted with a Dean-Stark trap for 26 hours. After cooling to room temperature, the solids are filtered off, and the filter cake is washed with 100 ml of xylene. The solvents are evaporated under reduced pressure to give an oil which is dissolved in a mixture of 50 g of silica gel in 750 ml of heptane. The solids are filtered off and the solvents are evaporated under reduced pressure to give N-(2′-chloro-4′,6′-difluorophenyl)-4-methylaniline as an oil.

後処理

  1. temperatureheated
  2. temperatureto reflux in a flask
  3. customfitted with a Dean-Stark trap for 26 hours
  4. filtrationthe solids are filtered off
  5. washthe filter cake is washed with 100 ml of xylene
  6. customThe solvents are evaporated under reduced pressure
  7. customto give an oil which
  8. filtrationThe solids are filtered off
  9. customthe solvents are evaporated under reduced pressure

出典と根拠

ORDレコード
ord-2c026e4d692947e2a345b16dae5aa2ae
出典データセット
uspto-grants-2006_10
特許番号
US07115662B2

反応ノート

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