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Hydrochloric Acid → Diethyl 5-amino-2-chloro-6-methylpyridine-3,4-dicarboxylate

HRID 37477
ノート
印刷プレビュー

反応式

HRID 37477 の反応式
[Cl:1][C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:5]([N+:18]([O-])=O)=[C:4]([CH3:21])[N:3]=1.Cl>C(O)C>[NH2:18][C:5]1[C:4]([CH3:21])=[N:3][C:2]([Cl:1])=[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[C:6]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 199355842-Chloro-3,4-diethoxycarbonyl-6-methyl-5-nitropyridine

生成物 1

HCID 15289693Diethyl 5-amino-2-chloro-6-methylpyridine-3,4-dicarboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 15 ml of ethanol was dissolved 1.2 g of 2-chloro-3,4-diethoxycarbonyl-6-methyl-5-nitropyridine, whereto 1.9 g (9 eq.) of reduced iron was added, followed by adding dropwise 7.1 ml of hydrochloric acid. The mixture was stirred at room temperature for 30 minutes. After the solvent was distilled off, the residue was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried. The solvent was distilled off to give an oily product.

後処理

  1. additionwas added
  2. distillationAfter the solvent was distilled off
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
  5. customdried
  6. distillationThe solvent was distilled off
  7. customto give an oily product

出典と根拠

ORDレコード
ord-85212bf9fa35470e9ef24fe3284c0ef7
出典データセット
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05420275

反応ノート

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