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Water → Ethyl 2,6-dichloro-4-methylnicotinate

HRID 1753904
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HRID 1753904 반응식
[Cl:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[C:6]([CH3:11])[CH:5]=[C:4]([Cl:12])[N:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:19](I)[CH3:20].O>CN(C)C=O>[CH2:19]([O:9][C:8]([C:7]1[C:2]([Cl:1])=[N:3][C:4]([Cl:12])=[CH:5][C:6]=1[CH3:11])=[O:10])[CH3:20]
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참가 물질

6

반응물 4

HCID 962WaterHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 6761212,6-Dichloro-4-methylpyridine-3-carboxylic acid

생성물 1

HCID 70700301Ethyl 2,6-dichloro-4-methylnicotinate수율 98.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2,6-dichlor-4-methylpyridin-3-carboxylic acid (100 g, 485 mmol) and potassium carbonate (100 g, 728 mmol) in dimethylformamide (1.25 I) is stirred for 30 h at RT before ethyl iodide (59.5 ml, 728 mmol) is added and stirring is continued for 18 h. After completion of the reaction, water is added and the mixture is extracted with ethyl acetate (3×). The combined organic layers are washed with water (2×) and brine (1×), dried over magnesium sulphate and evaporated to dryness to yield 2,6-dichloro-4-methyl-pyridine-3-carboxylic acid ethyl ester (112 g), which was used without further purification.

후처리

  1. additionis added
  2. additionis added
  3. extractionthe mixture is extracted with ethyl acetate (3×)
  4. washThe combined organic layers are washed with water (2×) and brine (1×)
  5. dry with materialdried over magnesium sulphate
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-28981a85e8064fbab441185c086ed825
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09168259B2

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