Ethanol → Ethyl 3-[2-(2-methoxyethoxy)-5-nitropyridin-4-yl]-2-oxopropionate potassium salt

HRID 553566노트

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HRID 553566 반응식
[K:1].CCO.[CH3:5][O:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[C:14]([CH3:16])[C:13]([N+:17]([O-:19])=[O:18])=[CH:12][N:11]=1.[C:20](OCC)(=[O:26])[C:21]([O:23][CH2:24][CH3:25])=[O:22]>C(OCC)C.C1(C)C=CC=CC=1>[K:1].[CH3:5][O:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[C:14]([CH2:16][C:20](=[O:26])[C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:13]([N+:17]([O-:19])=[O:18])=[CH:12][N:11]=1

참가 물질

7

반응물 4

HCID 702Ethanol2회HCID 7268Diethyl OxalateHCID 5462222PotassiumHCID 598200212-(2-Methoxyethoxy)-4-methyl-5-nitropyridine

생성물 1

HCID 67461922Ethyl 3-[2-(2-methoxyethoxy)-5-nitropyridin-4-yl]-2-oxopropionate potassium salt

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283Diethyl Ether용매2회

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온도
0 °C

실험 절차

1.86 g of potassium are initially charged in 120 ml of dry diethyl ether, and 15 ml of EtOH are added slowly. The mixture is cooled to 0° C. 5 g of 2-(2-methoxyethoxy)-4-methyl-5-nitropyridine are dissolved in 15 ml of dry ether and 3 ml of EtOH and added. 27.5 g of diethyl oxalate were dissolved in 100 ml of toluene and, at 0° C., added dropwise over a period of 45 min. The mixture is stirred at room temperature for 24 h. The precipitate is allowed to settle, the mixture is filtered and the precipitate is washed with ether/n-heptane 1:1. The precipitate is dried under high vacuum. This gives ethyl 3-[2-(2-methoxyethoxy)-5-nitropyridin-4-yl]-2-oxopropionate potassium salt as a red solid. (LC-MS protonate form) C13H16N2O7 (312.28), MS (ESI): 313 (M+H+).

후처리

  1. additionadded dropwise over a period of 45 min
  2. filtrationthe mixture is filtered
  3. washthe precipitate is washed with ether/n-heptane 1:1
  4. customThe precipitate is dried under high vacuum

출처 및 근거

ORD 기록
ord-93c2fb5a97904574b1b74696e84b3765
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08048901B2

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