Potassium Carbonate → HCID 67055245、化合物

HRID 601655

反応式

HRID 601655 の反応式
[CH3:1][NH:2][CH:3]([CH3:5])[CH3:4].C(=O)([O-])[O-].[K+].[K+].CN(C)S(=O)=O.Cl[C:19]1[CH:28]=[CH:27][C:26]2[C:21](=[CH:22][CH:23]=[C:24]([Br:29])[CH:25]=2)[N:20]=1>O>[Br:29][C:24]1[CH:25]=[C:26]2[C:21](=[CH:22][CH:23]=1)[N:20]=[C:19]([N:2]([CH3:1])[CH:3]([CH3:5])[CH3:4])[CH:28]=[CH:27]2

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 78485N-MethylisopropylamineHCID 128940866-Bromo-2-chloroquinolineHCID 178486088HCID 178486088、化合物

生成物 1

HCID 67055245HCID 67055245、化合物収率 2.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

Under nitrogen atmosphere, 180 mg of N-methylisopropylamine, and 200 g of potassium carbonate were added at room temperature sequentially to 5 ml solution of dimethylsulfonamide with 63 g of 2-chloro-6-bromoquinoline, and the mixture was stirred at 110° C. for 4 hours. Water was added to the reaction solution, extracted with ethyl acetate. Ethyl acetate layer was washed with saturated saline solution, and dried with anhydrous sodium sulfate. The solvents were distilled outunder reduced pressure, and the residues were separated and purified by silicagel chromatography (hexane/ethyl acetate=3/1) to obtain 18 mg of the above compound as a white solid.

後処理

  1. extractionextracted with ethyl acetate
  2. washEthyl acetate layer was washed with saturated saline solution
  3. dry with materialdried with anhydrous sodium sulfate
  4. distillationThe solvents were distilled outunder reduced pressure
  5. customthe residues were separated
  6. custompurified by silicagel chromatography (hexane/ethyl acetate=3/1)

出典と根拠

ORDレコード
ord-1c89321693754e3bb4331fa3b6b35c4c
出典データセット
uspto-grants-2011_03
特許番号
US07902369B2

関連ノート

読み込み中…