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Hydrochloric Acid → 1-[Bis(4-fluorophenyl)methyl]-4,6-dimethyl-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile

HRID 730433
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HRID 730433 반응식
[NH2:1][C:2]1[N:6]([CH:7]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)[CH:5]=[C:4]([C:22]#[N:23])[CH:3]=1.[C:24]([CH2:27][C:28](=O)[CH3:29])(=O)[CH3:25].Cl.C(=O)(O)[O-].[Na+]>C(O)C>[F:14][C:11]1[CH:10]=[CH:9][C:8]([CH:7]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[N:6]2[C:2]3=[N:1][C:24]([CH3:25])=[CH:27][C:28]([CH3:29])=[C:3]3[C:4]([C:22]#[N:23])=[CH:5]2)=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 31261AcetylacetoneHCID 516892Sodium BicarbonateHCID 230746485-Amino-1-[bis(4-fluorophenyl)methyl]-1H-pyrrole-3-carbonitrile

생성물 1

HCID 690625951-[Bis(4-fluorophenyl)methyl]-4,6-dimethyl-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile

시약·촉매·용매 1

HCID 702
Ethanol
용매

실험 절차

To a solution of 5-amino-1-[bis(4-fluorophenyl)methyl]-1H-pyrrole-3-carbonitrile (13.9 g, 45.1 mmol) in ethanol (200 ml) was sequentially added acetylacetone (5.02 g, 50.2 mmol) and concentrated hydrochloric acid (2.0 ml). The mixture was heated under reflux for 3 hours, poured into saturated sodium bicarbonate solution and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to give the objective product as a solid material.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 3 hours
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-b681d3b3533d4b5ca9ac20453ac36437
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582651B2

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