Ethyl Acrylate → 7-[[5-(2-Ethoxy-ethyl)-1,2,4-oxadiazol-3-yl]-methyl]-theophylline

HRID 1285168ノート

反応式

HRID 1285168 の反応式
[N:1]1([C:12](=[O:13])[C:11]2[N:10]([CH2:14][C:15](=[N:17][OH:18])[NH2:16])[CH:9]=[N:8][C:7]=2[N:5]([CH3:6])[C:3]1=[O:4])[CH3:2].[C:19]([O:23][CH2:24][CH3:25])(=O)[CH:20]=[CH2:21].CC[O-].[Na+]>C(O)C>[CH2:24]([O:23][CH2:19][CH2:20][C:21]1[O:18][N:17]=[C:15]([CH2:14][N:10]2[C:11]3[C:12](=[O:13])[N:1]([CH3:2])[C:3](=[O:4])[N:5]([CH3:6])[C:7]=3[N:8]=[CH:9]2)[N:16]=1)[CH3:25]

参加物

5

反応物 3

HCID 8821Ethyl AcrylateHCID 2723922Sodium ethoxideHCID 30574902-(Theophyllin-7-yl)-acetamidoxime

生成物 1

HCID 202499377-[[5-(2-Ethoxy-ethyl)-1,2,4-oxadiazol-3-yl]-methyl]-theophylline収率 95%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

12.6 g. 2-(theophyllin-7-yl)-acetamidoxime, 10 g. of ethyl acrylate, 220 cm3 of ethanol and 3.4 g. of sodium ethylate are heated under stirring for 15 hours. 16 g. (95% yield) of raw 7-[[5-(2-ethoxy-ethyl)-1,2,4-oxadiazol-3-yl]-methyl]-theophylline are obtained. This product is heated with 20 cm3 diethylamine under stirring for 8 hours on a 110° C. oil bath. The mixture is then evaporated at reduced pressure, washed by trituration with water and salt is formed with 5.8 g. of maleic acid in hot ethanol. 16.2 g. (68% yield) of 7-[{5-(2-diethylamino-ethan-1-yl)-1,2,4-oxadiazol-3-yl}-methyl]-theophilline-maleinate are are obtained. M.p.: 125°-128° C.

出典と根拠

ORDレコード
ord-5dd7d897c6de412d8202acab2f9d3303
出典データセット
uspto-grants-1986_01
特許番号
US04565817

反応ノート

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