Sodium Hydroxide → 2,6-Dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl ester

HRID 1496685

反応式

HRID 1496685 の反応式
[CH3:1][C:2]1[NH:3][C:4]([CH3:25])=[C:5]([C:21]([O:23]C)=[O:22])[CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[CH:13]=2)[C:7]=1[C:8]([O:10][CH3:11])=[O:9].[OH-].[Na+]>CO>[CH3:11][O:10][C:8]([C:7]1[CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[CH:13]=2)[C:5]([C:21]([OH:23])=[O:22])=[C:4]([CH3:25])[NH:3][C:2]=1[CH3:1])=[O:9]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 89082m-Nifedipine

生成物 1

HCID 1733222,6-Dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl ester収率 57.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

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%.

後処理

  1. customwas conducted at 70° C.
  2. stirringunder violent stirring for 6 hours
  3. customevaporated under reduced pressure
  4. customto remove 80 mL methanol
  5. additionTo the residue was added 200 mL water
  6. customThe unreacted starting materials are removed by filtration
  7. customto separate a yellow solid, which
  8. filtrationwas filtered
  9. customdried
  10. customto produce a khaki powder

出典と根拠

ORDレコード
ord-60c066ce929e440abb6a308e530d6fa5
出典データセット
uspto-grants-2015_12
特許番号
US09198902B2

関連ノート

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