HRID646672

反应详情

EQUATION

反应方程式

HRID 646672 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-amino-N-methyl-6-[4-(tetrahydro-2H-pyran-2-yloxy)phenyl]pyrazine-2-carboxamide (63 mg) was suspended in methanol followed by addition of aqueous hydrochloric acid (2 mL). The mixture was stirred for 15 min., poured into water (10 mL), and extracted with ethyl acetate (10 mL). The organic layer was washed with saturate aqueous sodium chloride then dried over anhydrous sodium sulfate. Filtration, concentration and column chromatography on silica followed by drying in vacuo afforded 3-amino-N-methyl-6-(4-hydroxyoxyphenyl)pyrazine-2-carboxamide (30 mg, 64% yield): 1H NMR (400 MHz; DMSO-D6): 9.62 (s, 1H); 8.78 (m, 1H); 8.82 (m, 1H); 8.7 (s, 1H); 7.98 (d, 2H); 7.5 (br s, 1H); 6.8 (d, 2H); 2.85 (d, 3H); MS (EI) for C12H12N4O2:245 (MH+).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (10 mL)
  2. washThe organic layer was washed with saturate aqueous sodium chloride
  3. dry with materialthen dried over anhydrous sodium sulfate
  4. filtrationFiltration, concentration and column chromatography on silica
  5. customby drying in vacuo