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

HRID 1787708

반응식

HRID 1787708 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1dda6433de5b4aab9845db9fde330951
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07511059B2

연결된 노트

불러오는 중…