[O:1]=[C:2]1[NH:7][C:6](=[S:8])[NH:5][C:4]([CH2:9][C:10]2[CH:11]=[C:12]3[C:17](=[CH:18][CH:19]=2)[C:16]([C:20]([OH:22])=[O:21])=[CH:15][CH:14]=[CH:13]3)=[CH:3]1.[OH-].[Na+].[CH3:25]I>C1COCC1.O>[OH:1][C:2]1[N:7]=[C:6]([S:8][CH3:25])[N:5]=[C:4]([CH2:9][C:10]2[CH:11]=[C:12]3[C:17](=[CH:18][CH:19]=2)[C:16]([C:20]([OH:22])=[O:21])=[CH:15][CH:14]=[CH:13]3)[CH:3]=12.30 g (7.37 mMol) 6-(6-oxo-2-thioxo-1,2,3,6-tetrahydro-pyrimidin-4-ylmethyl)-naphthalene-1-carboxylic acid are suspended in 160 ml THF. Then a solution of 452 mg (11.3 mMol) NaOH in 9 ml water is added, followed by 556 μl (8.93 mMol) methyliodide. After 15 h, the reaction mixture is concentrated in vacuo. The residue is used without further purification in Step 3.8. Pure title compound can be obtained by chromatography (Combi Flash; CH2Cl2→CH2Cl2/MeOH 7:1): TLC (CH2Cl2/MeOH 4:1): Rf=0.46.
読み込み中…
