Sodium Bicarbonate → Dimethyl 2-methyl-4-(2-nitrophenyl)-6-formyl-1,4-dihydropyridine-3,5-dicarboxylate

HRID 1248730ノート

反応式

HRID 1248730 の反応式
[CH3:1][C:2]1[NH:3][C:4]([CH:25](OC)[O:26]C)=[C:5]([C:21]([O:23][CH3:24])=[O:22])[CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[N+:18]([O-:20])=[O:19])[C:7]=1[C:8]([O:10][CH3:11])=[O:9].C(=O)(O)[O-].[Na+]>CC(C)=O.Cl>[CH3:1][C:2]1[NH:3][C:4]([CH:25]=[O:26])=[C:5]([C:21]([O:23][CH3:24])=[O:22])[CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[N+:18]([O-:20])=[O:19])[C:7]=1[C:8]([O:10][CH3:11])=[O:9]

参加物

5

反応物 2

HCID 516892Sodium BicarbonateHCID 12896948HCID 12896948、化合物

生成物 1

HCID 15737325Dimethyl 2-methyl-4-(2-nitrophenyl)-6-formyl-1,4-dihydropyridine-3,5-dicarboxylate収率 98.5%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒2 回HCID 313Hydrochloric Acid溶媒

反応条件

温度
25 °C

実験手順

A mixture of a solution of dimethyl 2-methyl-4-(2-nitrophenyl)-6-dimethoxymethyl-1,4-dihydropyridine-3,5-dicarboxylate (10.68 g) in acetone (110 ml) and 6N hydrochloric acid (10 ml) was stirred at 25° C. for 3 hours, which was neutralized with an aqueous sodium bicarbonate solution and acetone was distilled off under reduced pressure. The resultant reddish yellow oily precipitates were solidified, which were cracked finely, collected by filtration, washed with water and air dried over-night to give crude crystals of dimethyl 2-methyl-4-(2-nitrophenyl)-6-formyl-1,4-dihydropyridine-3,5-dicarboxylate (9.33 g).

後処理

  1. distillationwas distilled off under reduced pressure
  2. customThe resultant reddish yellow oily precipitates
  3. filtrationcollected by filtration
  4. washwashed with water and air
  5. customdried over-night

出典と根拠

ORDレコード
ord-973325ed84964349b0bab3c29f36d74b
出典データセット
uspto-grants-1985_06
特許番号
US04525478

反応ノート

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