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Ammonia → Ethyl 4-amino-6-chloro-5-nitronicotinate

HRID 1268831
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HRID 1268831 반응식
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([Cl:11])[N:5]=[C:4](C)[C:3]=1[C:13]([OH:15])=[O:14].[CH2:16](N(CC)CC)[CH3:17].[NH3:23].O1CCOCC1>ClCCl>[CH2:16]([O:15][C:13]([C:3]1[CH:4]=[N:5][C:6]([Cl:11])=[C:7]([N+:8]([O-:10])=[O:9])[C:2]=1[NH2:23])=[O:14])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 312751,4-DioxaneHCID 203278654,6-dichloro-2-methyl-5-nitro-3-Pyridinecarboxylic acid

생성물 1

HCID 45588416Ethyl 4-amino-6-chloro-5-nitronicotinate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4,6-Dichloro-2-methyl-5-nitro-pyridine-3-carboxylic acid (15 g, 56.6 mmol) and triethylamine (7.9 mL, 57.3 mmol) in dichloromethane (84 mL) at 0° C. was added dropwise ammonia solution in dioxane (0.5 M, 113 mL, 56.5 mmol). The mixture was then stirred overnight. Removal of the solvent followed by column chromatography gave 9 as a yellow crystalline solid. (7.3 g). 1H-NMR δ: 1.32 (t, J=7.1 Hz, 3H), 4.33 (q, J=7.1 Hz, 2H), 8.06 (s, br, 2H), 8.62 (s, 1H).

후처리

  1. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-a0d1c99674914fde8fc14542af2d2dbb
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07199119B2

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