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

HRID 730433
ノート
印刷プレビュー

反応式

HRID 730433 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b681d3b3533d4b5ca9ac20453ac36437
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07582651B2

反応ノート

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