反応 #321314

反応方程式

compound

[[4-[[[trans-4-(acetylaminomethyl)cyclohexyl]carbonylamino]acetyl]-o-phenylene]dioxy]diacetic acid disodium salt

triethylamine

4-cyanobenzoyl chloride

dimethylformamide

→

dimethyl [[4-[[[trans-4-[(p-cyanobenzoyl)aminomethyl]cyclohexyl]carbonylamino]acetyl]-o-phenylene]dioxy]diacetate

収率 62.0%

溶媒

chloroform

反応条件

後処理

1. 1
   濃縮After the reaction mixture was concentrated under reduced pressure
2. 2
   その他the residue thus obtained
3. 3
   洗浄washed with water
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   その他After the inorganic salt was removed by filtration
6. 6
   濃縮the filtrate was concentrated under reduced pressure
7. 7
   その他The solid product thus obtained
8. 8
   洗浄was washed with ether

実験手順

To the solution of 470 mg (0.83 mmole) of the compound prepared in Example 5 (a) in 5 ml of dimethylformamide were added 0.23 ml of triethylamine and 138 mg of 4-cyanobenzoyl chloride, and the mixture was stirred at room temperature for 1 hour. After the reaction mixture was concentrated under reduced pressure, the residue thus obtained was dissolved in chloroform, washed with water and dried over anhydrous magnesium sulfate. After the inorganic salt was removed by filtration, the filtrate was concentrated under reduced pressure. The solid product thus obtained was washed with ether to give 300 mg of dimethyl [[4-[[[trans-4-[(p-cyanobenzoyl)aminomethyl]cyclohexyl]carbonylamino]acetyl]-o-phenylene]dioxy]diacetate (yield, 62%).

出典