反应详情

To a 0° C. mixture of 5-Iodo-pyridine-2-thiol (904 mg, 3.81 mmol) in Methylene chloride (17 mL, 270 mmol) and Water (8.6 mL, 480 mmol) was added 37% hydrochloric acid (37:63, Hydrogen chloride:Water, 2.6 mL). 10% NaOCl (1:9, Sodium hypochlorite:Water, 2.0E1 mL) was then added dropwise over 10 min to the vigorously stirred reaction mixture. After stirring 20 min, the reaction mixture was partitioned, and the aqueous layer was extracted with methylene chloride (2×). The combined organic layers were washed with aqueous sodium bisulfite, dried over sodium sulfate, filtered and concentrated in vacuo to afford a light yellow crystalline solid.

1. customthe reaction mixture was partitioned
2. extractionthe aqueous layer was extracted with methylene chloride (2×)
3. washThe combined organic layers were washed with aqueous sodium bisulfite
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customto afford a light yellow crystalline solid