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

HRID 1164639ノート

反応式

HRID 1164639 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

7.09(1H, borad s), 7.35 to 7.85 (4H, m) 10.49 (1H, s). (b 4) 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 neutrallized 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-5f1a8e0de48341c5b327d1f3d4523ebf
出典データセット
uspto-grants-1983_01
特許番号
US04370334

反応ノート

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