反应详情

温度

80 °C

To a stirred suspension of N-(1,2,3,4-tetrahydro-5-isoquinolyl)methanesulfonamide hydrochloride prepared as described in Example 19(b) of WO 98/30560 (100 g, 0.38 mol) and 2-methyl-2-thiopseudourea sulfate (159 g, 0.57 mol) in water (1.5 liter) was added 2N aqueous sodium hydroxide (764 ml, 1.53 mol). The resulting solution was warmed to 80° C. and stirred at this temperature for 6 hours and then left to cool to room temperature overnight. Further 2-methyl-2-thiopseudourea sulfate (27 g, 0.10 mol) and 2N aq. sodium hydroxide (48 ml, 0.10 mol) were charged and the mixture heated at 80° C. for 1 hour. After this time the resulting suspension was cooled to room temperature, filtered, washed with water (1 liter) to give a white solid that was dried in vacuo overnight at 50° C. to give 91.0 g of the title product (89%).

1. customprepared
2. waitleft
3. temperatureto cool to room temperature overnight
4. temperaturethe mixture heated at 80° C. for 1 hour
5. temperatureAfter this time the resulting suspension was cooled to room temperature
6. filtrationfiltered
7. washwashed with water (1 liter)
8. customto give a white solid
9. customthat was dried in vacuo overnight at 50° C.