HRID1589423
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In a 250 ml round bottomed flask is placed 90 ml of N,N-dimethylformamide and 30 grams (0.092 mole) of 3-amino sulfonyl-4-chlorobenzhydrazide. The mixture was stirred to dissolve the solid, then 18.63 gms (0.138 mole) of crotyl bromide were added. The mixture was heated at 100° for 1.66 hours at which point TLC showed the reaction to be complete. The reaction mixture was cooled and diluted with 200 ml isopropanol. This solution was dripped into a slurry of 1.5 liters of ice and 4 liters of water. The solid which precipitated was collected, washed with water and air dried overnight, yielding the product which could be recrystallized from chloroform/carbon tetrachloride.
WORKUP
后处理
- customIn a 250 ml round bottomed flask is placed
- dissolutionto dissolve the solid
- temperatureThe mixture was heated at 100° for 1.66 hours at which point TLC
- customthe reaction
- temperatureThe reaction mixture was cooled
- customThe solid which precipitated
- customwas collected
- washwashed with water and air
- customdried overnight
- customyielding the product which
- customcould be recrystallized from chloroform/carbon tetrachloride