Tert-Butylamine → HCID 66836579、化合物

HRID 1631145ノート

反応式

HRID 1631145 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+].[C:18]([NH2:22])([CH3:21])([CH3:20])[CH3:19]>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][NH:22][C:18]([CH3:21])([CH3:20])[CH3:19]

参加物

5

反応物 3

HCID 6385Tert-ButylamineHCID 10796Cesium carbonateHCID 66836706HCID 66836706、化合物

生成物 1

HCID 66836579HCID 66836579、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 123 μl of tert-butylamine 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-d693cff4f76b4dff82bf24152fc3bba8
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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