反应详情

To a solution of 2.0 g of 1,8-naphthosultam in 7 mL of dimethoxyethane was added dropwise under gentle reflux a solution of 11.5 mL of sodium bis(2-methoxyethoxy)aluminum hydride in toluene (3.4 mol solution in toluene) over a period of 15 minutes, then stirred at reflux for 17 hours. The mixture was cooled in an ice-bath, 5 mL of water were added dropwise then the solution was neutralized with 4N sulfuric acid (pH~7) and extracted with ether (3×75 mL). The combined ether solutions were washed with water (75 mL) then dried (magnesium sulfate) and removal of the solvent gave 1.5 g of 8 -amino-1-napthalenethiol. The thiol was recrystallized from ether--petroleum ether to afford 1.3 g of 8-amino-1-naphthalenethiol, mp. 69°-72°.

1. temperatureat reflux for 17 hours
2. temperatureThe mixture was cooled in an ice-bath
3. extractionextracted with ether (3×75 mL)
4. washThe combined ether solutions were washed with water (75 mL)
5. customthen dried
6. custom(magnesium sulfate) and removal of the solvent