Sodium Iodide → HCID 22707973、化合物

HRID 353214ノート

反応式

HRID 353214 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[NH:11][C:10](=[O:12])[C:9]([C:13]#[N:14])=[CH:8][CH:7]=1.Cl[CH2:16][C:17]([NH2:19])=[O:18].[I-].[Na+].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.C(OCC)(=O)C.O>[C:13]([C:9]1[C:10]([O:12][CH2:16][C:17]([NH2:19])=[O:18])=[N:11][C:6]([C:2]2[O:1][CH:5]=[CH:4][CH:3]=2)=[CH:7][CH:8]=1)#[N:14]

参加物

8

反応物 4

HCID 5238Sodium IodideHCID 6580ChloroacetamideHCID 11430Potassium CarbonateHCID 27470886-(Furan-2-yl)-2-oxo-1,2-dihydropyridine-3-carbonitrile

生成物 1

HCID 22707973HCID 22707973、化合物収率 54%

試薬・触媒・溶媒 3

HCID 180Acetone溶媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

A suspension of 6-(2-furyl)-2-oxo-1,2-dihydro-3-pyridinecarbonitrile (6.0 g, 32.3 mmol), 2-chloroacetamide (3.0 g, 37.7 mmol), sodium iodide (5.7 g, 38.0 mmol) and potassium carbonate (9.0 g, 56.2 mmol) in acetone (100 ml) was stirred at 60° C. for 6 hours. After cooling as it was, the reaction solution was diluted with ethyl acetate and water. The organic layer was washed with an aqueous saturated solution of sodium bicarbonate (×2) and an aqueous saturated solution of ammonium chloride, dried over anhydrous sodium sulfate, and concentrated. Diethyl ether was added to the residue, and the resulting precipitates were collected by filtration and washed with diethyl ether, to give the title compound (4.2 g, 54%) as a brown solid.

後処理

  1. temperatureAfter cooling as it
  2. washThe organic layer was washed with an aqueous saturated solution of sodium bicarbonate (×2)
  3. dry with materialan aqueous saturated solution of ammonium chloride, dried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. additionDiethyl ether was added to the residue
  6. customthe resulting precipitates
  7. filtrationwere collected by filtration
  8. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-569a59fcda26478c847ca0dbbecc57a7
出典データセット
uspto-grants-2004_06
特許番号
US06750232B2

反応ノート

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