Methyl Lactate → 2-{1-(Methoxycarbonyl)ethoxy}-3-nitropyridine

HRID 1241306노트

반응식

HRID 1241306 반응식
[H-].[Na+].Cl[C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][N:5]=1.[C:13]([O:18][CH3:19])(=[O:17])[CH:14]([CH3:16])[OH:15]>O1CCOCC1>[CH3:19][O:18][C:13]([CH:14]([O:15][C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][N:5]=1)[CH3:16])=[O:17]

참가 물질

5

반응물 3

HCID 11040Methyl LactateHCID 24758Sodium hydrideHCID 796132-Chloro-3-nitropyridine

생성물 1

HCID 219335712-{1-(Methoxycarbonyl)ethoxy}-3-nitropyridine수율 73%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

First, 0.8 g of sodium hydride was added to a mixture of 3.17 g of 2-chloro-3-nitropyridine, 2.19 g of methyl lactate, and 20 ml of 1,4-dioxane at 10° C., and the mixture was stirred at room temperature for 1.5 hours. The reaction mixture was poured into ice water, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and then concentrated. The residue was subjected to silica gel column chromatography to give 3.3 g of 2-{1-(methoxycarbonyl)ethoxy}-3-nitropyridine.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fe2892fc00734084ba6f7361bf41b06c
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07115544B2

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