Potassium Cyanide → HCID 57998826, 화합물

HRID 1512070노트

반응식

HRID 1512070 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 57998826HCID 57998826, 화합물수율 100.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4a7eea5143434508a8be083b4908efc9
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217055B2

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