HRID256885
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
2,6-Diiodopyrazine (12 g, 36.14 mmol) was added to a solution of sodium (0.83 g, 36.10 mmol) in ethanol (75 ml). The solution was refluxed for 1 h, the solvent removed under vacuum, water (40 ml) added and extracted into dichloromethane (4×200 ml). The solvent was removed under vacuum and the residue chromatographed through silica-gel using dichloromethane as eluant to give 2-iodo-6-ethoxy pyrazine (6.5 g). m.p. 36°-37° C.; δ (60 MHz, CDCl3) 1.30 (3H, t, J=7 Hz, Me); 4.35 (2H, q, J=7 Hz, CH2Me); 8.07 (1H, s, pyrazine-H): 8.35 (1H, s, pyrazine-H).
WORKUP
后处理
- temperatureThe solution was refluxed for 1 h
- customthe solvent removed under vacuum, water (40 ml)
- additionadded
- extractionextracted into dichloromethane (4×200 ml)
- customThe solvent was removed under vacuum
- customthe residue chromatographed through silica-gel