反应详情

To a round bottom flask equipped with a magnetic stirrer and condenser were added 1.1 g (3.3 mmol) of dimethyl-sulfamic acid 5-tert-butyl-2-methyl-4-thiocyanato-phenyl ester (prepared in Example SSS), dithiothreitol (1.29 g, 8.35 mmol), EtOH (40 mL), and 0.02M KH2PO4 buffer solution (5 mL), respectively. The reaction was refluxed overnight. The mixture was then quenched with H2O (250 mL) and extracted with a 1:1 mixture of hexanes:Et2O. The organic layer was again washed with H2O and brine, dried (MgSO4) and concentrated. The residue was dried under high vacuum to yield the title compound. 1H NMR (CDCl3) δ 1.45 (s, 9 H), 2.25 (s, 3 H), 3.02 (s, 6 H), 3.57 (s, 1 H), 7.01 (s, 1 H), 7.28 (s, 1 H).

1. customTo a round bottom flask equipped with a magnetic stirrer and condenser
2. temperatureThe reaction was refluxed overnight
3. customThe mixture was then quenched with H2O (250 mL)
4. extractionextracted with a 1:1 mixture of hexanes
5. washThe organic layer was again washed with H2O and brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated
8. customThe residue was dried under high vacuum