2,6-Diaminopyridine → N-(6-Amino-pyridin-2-yl)-2-(2-methoxy-ethoxy)-acetamide

HRID 1787708

反応式

HRID 1787708 の反応式
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][C:7]([OH:9])=O.ClC(OCC(C)C)=O.[NH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([NH2:25])[N:20]=1.C(=O)(O)[O-].[Na+]>O1CCCC1.C(N(CC)CC)C>[NH2:18][C:19]1[N:20]=[C:21]([NH:25][C:7](=[O:9])[CH2:6][O:5][CH2:4][CH2:3][O:2][CH3:1])[CH:22]=[CH:23][CH:24]=1

参加物

7

反応物 4

HCID 88612,6-DiaminopyridineHCID 27642(2-Methoxyethoxy)acetic acidHCID 62365Isobutyl chloroformateHCID 516892Sodium Bicarbonate

生成物 1

HCID 57600508N-(6-Amino-pyridin-2-yl)-2-(2-methoxy-ethoxy)-acetamide

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒

反応条件

温度
0 °C

実験手順

4.9 ml of (2-methoxyethoxy)-acetic acid is dissolved in 500 ml of tetrahydrofuran. 9.7 ml of triethylamine and 5.6 ml of isobutyl chloroformate are added at 0° C., and it is stirred for 30 minutes at 0° C. 3.96 g of 2,6-diaminopyridine is added, and it is stirred for another 4 hours at room temperature. The reaction mixture is mixed with semi-saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic solution is washed with saturated sodium chloride solution, dried on sodium sulfate, concentrated by evaporation, and after purification by chromatography on silica gel, 5.04 g of the title compound is obtained.

後処理

  1. stirringit is stirred for another 4 hours at room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic solution is washed with saturated sodium chloride solution
  4. customdried on sodium sulfate
  5. concentrationconcentrated by evaporation
  6. customafter purification by chromatography on silica gel

出典と根拠

ORDレコード
ord-1dda6433de5b4aab9845db9fde330951
出典データセット
uspto-grants-2009_03
特許番号
US07511059B2

関連ノート

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