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

HRID 1285168노트

반응식

HRID 1285168 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

출처 및 근거

ORD 기록
ord-5dd7d897c6de412d8202acab2f9d3303
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04565817

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