反応 #1583867

反応方程式

dimethyl 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate

NaOH

→

title product

収率 57.2%

5-methoxycarbonyl-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylic acid

収率 57.2%

溶媒

methanol

methanol

反応条件

後処理

1. 1
   その他was conducted at 70° C.
2. 2
   workup.STIRRINGunder violent stirring for 6 hours
3. 3
   その他evaporated under reduced pressure
4. 4
   その他to remove 80 mL methanol
5. 5
   workup.ADDITIONTo the residue was added 200 mL water
6. 6
   その他The unreacted starting materials are removed by filtration
7. 7
   その他to separate a yellow solid, which
8. 8
   ろ過was filtered
9. 9
   その他dried
10. 10
    その他to produce a khaki powder

実験手順

3.5 g dimethyl 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate (0.01 mol) and 150 mL methanol were mixed. To the mixture was added a saturated aqueous NaOH solution (9 g, 0.225 mol) under stirring. The reaction was conducted at 70° C. under violent stirring for 6 hours, and evaporated under reduced pressure to remove 80 mL methanol. To the residue was added 200 mL water. The unreacted starting materials are removed by filtration. The filtrate was adjusted to a pH of about 2.5 with 1 mol/L hydrochloric acid to separate a yellow solid, which was filtered and dried to produce a khaki powder. The resulting powder was treated with methanol to produce the title product as a yellow solid (1.9 g) in a yield of 57.2%.

出典