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

HRID 1753904
ノート
印刷プレビュー

反応式

HRID 1753904 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 70700301Ethyl 2,6-dichloro-4-methylnicotinate収率 98.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-28981a85e8064fbab441185c086ed825
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09168259B2

反応ノート

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