Potassium Cyanide → HCID 57998826、化合物

HRID 1512070ノート

反応式

HRID 1512070 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[C:4]([CH2:9]Br)[C:3]=1[Cl:11].[C-:12]#[N:13].[K+]>C(O)C.O>[Br:1][C:2]1[C:3]([Cl:11])=[C:4]([CH2:9][C:12]#[N:13])[C:5]([F:8])=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 9032Potassium CyanideHCID 579988441-Bromo-3-(bromomethyl)-2-chloro-4-fluorobenzene

生成物 1

HCID 57998826HCID 57998826、化合物収率 100.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A solution of 1-bromo-3-bromomethyl-2-chloro-4-fluoro-benzene (9.945 g) (Example 4.2) in absolute ethanol (40 ml) was added dropwise to a solution of potassium cyanide (2.38 g) in water (2 ml) under heating over a period of 30 minutes. The reaction mixture was heated to reflux for 7 hours. The reaction mixture was then allowed to cool to ambient temperature and then stored at ambient temperature for 16 hours. The mixture was filtered and the filtrate concentrated. The residue was dissolved in ethyl acetate, dried over magnesium sulfate and concentrated to give (3-bromo-2-chloro-6-fluoro-phenyl)-acetonitrile as a pale yellow oil (8.19 g). 1H-NMR (400 MHz, CDCl3): 3.89 (d, 2H), 7.00 (t, 1H), 7.64 (dd, 1H) ppm.

後処理

  1. temperatureunder heating over a period of 30 minutes
  2. temperatureThe reaction mixture was heated
  3. temperatureto reflux for 7 hours
  4. filtrationThe mixture was filtered
  5. concentrationthe filtrate concentrated
  6. dissolutionThe residue was dissolved in ethyl acetate
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-4a7eea5143434508a8be083b4908efc9
出典データセット
uspto-grants-2012_07
特許番号
US08217055B2

反応ノート

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