反应详情

温度

100 °C

To a stirred solution of 9-2 (5 g, 8.9 mMol) in anhydrous 1,4-dioxane (20 mL) was added hydrazine (5.9 mL, 188.1 mMol). The solution was heated to 100° C. in a microwave reactor for 5 minutes. The solvent was removed in vacuo and was dried azeotropically with toluene three times. The crude solid was triturated with a saturated NaHCO3 solution for 20 minutes. The suspension was filtered and washed with copious amounts of water. The solid was dried azeotropically with toluene three times to yield 9-3 as a tan solid. LC/MS (M+1) calculated: 554.6; observed: 554.2

1. customThe solvent was removed in vacuo
2. dry with materialwas dried azeotropically with toluene three times
3. customThe crude solid was triturated with a saturated NaHCO3 solution for 20 minutes
4. filtrationThe suspension was filtered
5. washwashed with copious amounts of water
6. dry with materialThe solid was dried azeotropically with toluene three times