Cesium carbonate → HCID 66836638、化合物

HRID 1631151ノート

反応式

HRID 1631151 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[CH2:10]Cl.C(=O)([O-])[O-].[Cs+].[Cs+].[CH3:18][CH:19]1[CH2:23][CH2:22][CH:21]([CH3:24])[NH:20]1>C(#N)C>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[CH2:10][N:20]1[CH:21]([CH3:24])[CH2:22][CH2:23][CH:19]1[CH3:18]

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 960342,5-DimethylpyrrolidineHCID 66836706HCID 66836706、化合物

生成物 1

HCID 66836638HCID 66836638、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

200 mg of 1-bromo-2-chloromethyl-4,5-difluorobenzene are dissolved in 5 ml of acetonitrile. 540 mg of caesium carbonate and 152 μl of 2,5-dimethylpyrrolidine are added, and the mixture is stirred at 80° C. for 16 h. After cooling to 25° C., the mixture is filtered, and the filtrate is evaporated to dryness. The residue is taken up in 5 ml of ethyl acetate, the solution is washed with 5 ml of 2N sodium hydroxide solution, and the combined organic phases are dried over sodium sulfate. After filtration, the filtrate is evaporated to dryness, after which the product is isolated as oil.

後処理

  1. temperatureAfter cooling to 25° C.
  2. filtrationthe mixture is filtered
  3. customthe filtrate is evaporated to dryness
  4. washthe solution is washed with 5 ml of 2N sodium hydroxide solution
  5. dry with materialthe combined organic phases are dried over sodium sulfate
  6. filtrationAfter filtration
  7. customthe filtrate is evaporated to dryness
  8. customafter which the product is isolated as oil

出典と根拠

ORDレコード
ord-ec84a88e47434fcb99fdbd4701c2896a
出典データセット
uspto-grants-2014_07
特許番号
US08791129B2

反応ノート

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