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

HRID 37477
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HRID 37477 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-85212bf9fa35470e9ef24fe3284c0ef7
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05420275

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