Water → 2-Amino-6-(2-furyl)-5-(4-propyl-3-pyridyl)-3-pyridinecarbonitrile

HRID 353230ノート

反応式

HRID 353230 の反応式
[NH2:1][C:2]1[N:9]=[C:8]([C:10]2[O:11][CH:12]=[CH:13][CH:14]=2)[C:7]([C:15]2[CH:20]=[CH:19][C:18](=O)[NH:17][CH:16]=2)=[CH:6][C:3]=1[C:4]#[N:5].C(=O)([O-])[O-].[K+].[K+].[CH2:28](I)[CH2:29][CH3:30].O>CN(C)C=O>[NH2:1][C:2]1[C:3]([C:4]#[N:5])=[CH:6][C:7]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][C:20]=2[CH2:28][CH2:29][CH3:30])=[C:8]([C:10]2[O:11][CH:12]=[CH:13][CH:14]=2)[N:9]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 99654582-Amino-6-(2-furyl)-5-(6-oxo-1,6-dihydro-3-pyridinyl)nicotinonitrile

生成物 1

HCID 227080532-Amino-6-(2-furyl)-5-(4-propyl-3-pyridyl)-3-pyridinecarbonitrile収率 11.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

2-Amino-6-(2-furyl)-5-(6-oxo-1,6-dihydro-3-pyridinyl)nicotinonitrile (20 mg, 0.072 mmol) and potassium carbonate (30 mg, 0.22 mmol) were introduced into a reaction vessel, dissolved in N,N-dimethylformamide (1 mL). Propyl iodide (52 mg, 0.31 mmol) was added thereto, followed by stirring at 70° C. for 18 hours. After the reaction was finished, water was added thereto, and it was extracted with ethyl acetate. After removing the aqueous layer, the organic layer was concentrated and purified by high performance liquid chromatography, to give the title product as a yellow solid (2.6 mg, 11%; 1.8 mg, 7.8%).

後処理

  1. extractionit was extracted with ethyl acetate
  2. customAfter removing the aqueous layer
  3. concentrationthe organic layer was concentrated
  4. custompurified by high performance liquid chromatography

出典と根拠

ORDレコード
ord-de97b6d598a847c5be3c3f6f9ddab0ac
出典データセット
uspto-grants-2004_06
特許番号
US06750232B2

反応ノート

読み込み中…