反応 #56063

反応方程式

methanol

cyclopropanecarboxylic acid

cyclopropanecarboxylic acid chloride

5-[1-hydroxy-2-(3,4-dimethoxyphenethylamino)ethyl]-8-hydroxycarbostyril hydrochloride

→

5-[1-cyclopropylcarbonyloxy-2-(3,4-dimethoxyphenethylamino)ethyl]-8-cyclopropylcarbonyloxycarbostyril hydrochloride

溶媒

diethyl ether

反応条件

後処理

1. 1
   その他to react for 1 hour at a temperature of 80° C
2. 2
   workup.ADDITIONwas added to the reaction mixture
3. 3
   その他to crystallize the product
4. 4
   その他The crystals thus obtained
5. 5
   その他were separated by filtration
6. 6
   洗浄washed with diethyl ether
7. 7
   その他recrystallized from a mixture of ethanol and acetone

実験手順

2 ml of cyclopropanecarboxylic acid and 1 ml of cyclopropanecarboxylic acid chloride were added to 500 mg of 5-[1-hydroxy-2-(3,4-dimethoxyphenethylamino)ethyl]-8-hydroxycarbostyril hydrochloride, and the mixture was allowed to react for 1 hour at a temperature of 80° C. After completion of the reaction, 10 ml of methanol was added to the reaction mixture while cooling with ice-water followed by addition of diethyl ether to crystallize the product. The crystals thus obtained were separated by filtration, washed with diethyl ether and recrystallized from a mixture of ethanol and acetone to obtain 210 mg of 5-[1-cyclopropylcarbonyloxy-2-(3,4-dimethoxyphenethylamino)ethyl]-8-cyclopropylcarbonyloxycarbostyril hydrochloride having a melting point of 167°-168° C. (with decomposition).

出典