Potassium Carbonate → HCID 59164777、化合物

HRID 1441726

反応式

HRID 1441726 の反応式
F[C:2]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:3]=1[CH:4]=O.Cl.[C:14]([NH2:17])(=[NH:16])[CH3:15].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[CH3:15][C:14]1[N:17]=[CH:4][C:3]2[C:2](=[CH:9][C:8]([N+:10]([O-:12])=[O:11])=[CH:7][CH:6]=2)[N:16]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 67170Acetamidine monohydrochlorideHCID 45629192-Fluoro-4-nitrobenzaldehyde

生成物 1

HCID 59164777HCID 59164777、化合物収率 34.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
25 °C

実験手順

2-Fluoro-4-nitrobenzaldehyde (1.00 g, 5.92 mmol) and acetamidine hydrochloride (0.783 g, 8.28 mmol) were added to a suspension of activated 4 Å MS (1.2 g) in acetonitrile (60 mL). K2CO3 (1.14 g, 8.28 mmol) was then added and the reaction was heated to reflux for 4 h. The reaction was then cooled to 25° C. and filtered through celite rinsing with CH2Cl2. The crude product was purified by flash chromatography on silica eluting with 0-10% acetone in CH2Cl2 to give 0.386 g of compound 25A as a yellow solid.

後処理

  1. temperaturethe reaction was heated
  2. temperatureto reflux for 4 h
  3. filtrationfiltered
  4. washthrough celite rinsing with CH2Cl2
  5. customThe crude product was purified by flash chromatography on silica eluting with 0-10% acetone in CH2Cl2

出典と根拠

ORDレコード
ord-6049b3b6053640fbb4e80b2dc4f7fbbb
出典データセット
uspto-grants-2010_02
特許番号
US07655688B2

関連ノート

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