Tetrahydrofuran → HCID 59385070、化合物

HRID 2356747ノート

反応式

HRID 2356747 の反応式
Cl.Cl.[NH2:3][CH2:4][C:5]([C:7]1[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=1)=[O:6].[F:13][C:14]1[CH:22]=[CH:21][C:17]([C:18](Cl)=[O:19])=[CH:16][CH:15]=1.C(=O)([O-])O.[Na+].O1CCCC1>C(OCC)(=O)C.O>[F:13][C:14]1[CH:22]=[CH:21][C:17]([C:18]([NH:3][CH2:4][C:5]([C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)=[O:6])=[O:19])=[CH:16][CH:15]=1

参加物

7

反応物 4

HCID 8028TetrahydrofuranHCID 678794-Fluorobenzoyl chlorideHCID 516892Sodium BicarbonateHCID 190185823-(2'-Aminoacetyl)pyridine dihydrochloride

生成物 1

HCID 59385070HCID 59385070、化合物収率 66.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 3-(2-aminoacetyl)pyridine dihydrochloride (50.00 g), 4-fluorobenzoylchloride (41.71 g) and sodium hydrogen carbonate (100.44 g) in ethyl acetate (1 liter) and water (0.6 liter) was stirred at room temperature for 2 hours. To the reaction mixture were added tetrahydrofuran (0.5 liter) and water (1 liter), and the organic layer was collected. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and the solvent was removed under reduced pressure. The resulting residue was triturated with ethyl acetate to obtain 3-[2-(4-fluorobenzoyl)aminoacetyl]pyridine (40.87 g) as pale yellowish powder.

後処理

  1. customthe organic layer was collected
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was removed under reduced pressure
  5. customThe resulting residue was triturated with ethyl acetate

出典と根拠

ORDレコード
ord-6496f246c6bb435aac00c0cc5267eb98
出典データセット
uspto-grants-2010_07
特許番号
US07759373B2

反応ノート

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