Sodium Carbonate → 5-(Aminomethyl)-2-fluorobenzonitrile

HRID 1093042노트

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HRID 1093042 반응식
Br[CH2:2][C:3]1[CH:4]=[CH:5][C:6]([F:11])=[C:7]([CH:10]=1)[C:8]#[N:9].[NH3:12].CO.C([O-])([O-])=O.[Na+].[Na+]>CCOCC>[NH2:12][CH2:2][C:3]1[CH:4]=[CH:5][C:6]([F:11])=[C:7]([CH:10]=1)[C:8]#[N:9]

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 27739315-(Bromomethyl)-2-fluorobenzonitrileHCID 21705897Ammonia methanol

생성물 1

HCID 186161975-(Aminomethyl)-2-fluorobenzonitrile

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A solution of 5-(bromomethyl)-2-fluorobenzonitrile (300 mg, 1.402 mmol) in 7M NH3/methanol (5 mL, 35.0 mmol) was stirred at room temp for 18 h. After the removing the solvent the resulting residue was stirred with Et2O/sat. Na2CO3. The aqueous layer was then separated and the organic layer dried (Na2SO4), filtered and concentrated to give a 3:1 mixture of the title compound, amine 5-(aminomethyl)-2-fluorobenzonitrile contaminated and 5,5′-azanediylbis(methylene)bis(2-fluorobenzonitrile). The mixture was used without further purification. 1H NMR (500 MHz, CDCl3) δ: 7.48-7.66 (2 H, m), 7.07-7.21 (1 H, m), 3.89 (2 H, s).

후처리

  1. customThe aqueous layer was then separated
  2. dry with materialthe organic layer dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto give

출처 및 근거

ORD 기록
ord-f3bc8adda5f14964a364c3d14be695e0
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129398B2

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