Potassium Carbonate → HCID 58853204、化合物

HRID 1943774ノート

反応式

HRID 1943774 の反応式
F[C:2](F)(F)[C:3]1[CH:8]=[CH:7][C:6]([CH:9]([NH2:13])[CH2:10][CH2:11][CH3:12])=[CH:5][CH:4]=1.[Cl:16][C:17]1[CH:22]=[N:21][CH:20]=[C:19](Cl)[N:18]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.C(OCC)(=O)C.O>[Cl:16][C:17]1[N:18]=[C:19]([NH:13][CH:9]([C:6]2[CH:7]=[CH:8][C:3]([CH3:2])=[CH:4][CH:5]=2)[CH2:10][CH2:11][CH3:12])[CH:20]=[N:21][CH:22]=1

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 785042,6-DichloropyrazineHCID 59339521HCID 59339521、化合物

生成物 1

HCID 58853204HCID 58853204、化合物収率 5.7%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 1-[4-(trifluoromethyl)phenyl]butan-1-amine (0.40 g, 1.9 mmol) and 2,6-dichloropyrazine (0.55 g, 3.7 mmol) in 1,4-dioxane (6 mL) was added anhydrous potassium carbonate (0.39 g, 2.8 mmol). The resulting mixture was heated at reflux for 18 h. After cooling to room temperature, the mixture was diluted with ethyl acetate and H2O. The organic phase was collected, dried and concentrated. The residue was purified by flash chromatography eluting with ethyl acetate-hexane (1:1) to give pure product (0.03 g, 5%).

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 18 h
  3. customThe organic phase was collected
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by flash chromatography
  7. washeluting with ethyl acetate-hexane (1:1)

出典と根拠

ORDレコード
ord-ee4653b2ac7848dcb2f02208739a7bcd
出典データセット
uspto-grants-2013_03
特許番号
US08394806B2

反応ノート

読み込み中…