Potassium Iodide → 2-Iodomethyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine

HRID 1904580

反応式

HRID 1904580 の反応式
Cl[CH2:2][C:3]1[NH:4][C:5]([CH3:28])=[C:6]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10].[I-:29].[K+]>CC(C)=O>[I:29][CH2:2][C:3]1[NH:4][C:5]([CH3:28])=[C:6]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10]

参加物

4

反応物 2

HCID 4875Potassium IodideHCID 3064723Diethyl 2-(chloromethyl)-6-methyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate

生成物 1

HCID 200374752-Iodomethyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine収率 36%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 2-chlorometyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine (0.5 g) and potassium iodide (1 g) in acetone (5 ml) is stirred at room temperature for 24 hours, then it is filtered, concentrated under reduced pressure and the residue purified by column chromatography on silica gel (20 g, eluent: hexane/AcOEt 80/20) to give 0.22 g of 2-iodomethyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine as an oil.

後処理

  1. filtrationit is filtered
  2. concentrationconcentrated under reduced pressure
  3. customthe residue purified by column chromatography on silica gel (20 g, eluent: hexane/AcOEt 80/20)

出典と根拠

ORDレコード
ord-9b3be743995741288858057a4df6200a
出典データセット
uspto-grants-1989_06
特許番号
US04839348

関連ノート

読み込み中…