反応 #353890

反応方程式

acetic anhydride

methyl acetate

methyl 6-amino-5-cyano-4-(2,3-dichlorophenyl)-2-methyl-1,4-dihydropyridine-3-carboxylate

acetic anhydride

→

Methyl 6-acetamido-5-cyano-4-(2,3-dichlorophenyl)-2-methyl-l,4-dihydropyridine-3-carboxylate

溶媒

methanol

反応条件

後処理

1. 1
   温度under reflux for 30 minutes
2. 2
   その他The reaction solution is evaporated in vacuo and toluene
3. 3
   その他The crystals which have separated out
4. 4
   ろ過are filtered off
5. 5
   洗浄washed with toluene

実験手順

6.7 g (20 mmol) of methyl 6-amino-5-cyano-4-(2,3-dichlorophenyl)-2-methyl-1,4-dihydropyridine-3-carboxylate and 33.5 ml (350 mmol) of acetic anhydride are heated under reflux for 30 minutes. Excess acetic anhydride is then converted into methyl acetate by addition of methanol at 25° C., while stirring. The reaction solution is evaporated in vacuo and toluene is then shipped off from the residue twice in vacuo. The residue is then boiled up with 50 ml of toluene. The crystals which have separated out are filtered off and washed with toluene.

出典