Ethanolamine → N-(2-Hydroxyethyl)picolinamide

HRID 34950

反応式

HRID 34950 の反応式
[CH2:1]([CH2:3][NH2:4])[OH:2].[N:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](Cl)=[O:12]>CN(C)C=O>[OH:2][CH2:1][CH2:3][NH:4][C:11]([C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][N:5]=1)=[O:12]

参加物

4

反応物 2

HCID 700EthanolamineHCID 135034Pyridine-2-carbonyl chloride

生成物 1

HCID 2045999N-(2-Hydroxyethyl)picolinamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

15.4 ml of ethanolamine were placed under argon with 30 ml of dimethylformamide and cooled to 0°-5°. A solution of 11.3 g of picolinic acid chloride in 100 ml of dimethylformamide was added dropwise thereto at 0°-10° and the mixture was stirred at room temperature overnight. The dimethylformamide was distilled off under reduced pressure. The residue was dissolved in methylene chloride and separated from the insoluble constituents, and thereafter chromatographed on silica gel; elution agent: methylene chloride, thereafter methylene chloride/methanol (9:1). N-(2-Hydroxyethyl)pyridine-2-carboxamide was obtained as a yellow oil.

後処理

  1. temperaturecooled to 0°-5°
  2. distillationThe dimethylformamide was distilled off under reduced pressure
  3. dissolutionThe residue was dissolved in methylene chloride
  4. customseparated from the insoluble constituents
  5. customchromatographed on silica gel
  6. washelution agent

出典と根拠

ORDレコード
ord-73ec8076ef72413595d304b362e40316
出典データセット
uspto-grants-1988_08
特許番号
US04764522

関連ノート

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