反应详情

温度

40 °C

To 15 g. (41.5 m moles) 4-(hexadecylamino)benzoic acid in 200 ml. warm chloroform is added 15 g. sodium carbonate in 150 ml. water. To the vigorously stirred solution is added 10 g. (59 m moles) carbobenzyloxy chloride. After 2 hours stirring at 40° C., the layers are separated, washed three times with 1 N hydrochloric acid, dried, and evaporated to an oil. The oil is dissolved in 300 ml. toluene, treated with 15 ml. (5 eq) thionyl chloride and the solution is refluxed for 5 hours. The solvents are evaporated and the residue is dissolved three times in toluene, evaporating each time to yield a viscous, orange oil.

1. additionTo the vigorously stirred solution is added 10 g
2. customthe layers are separated
3. washwashed three times with 1 N hydrochloric acid
4. customdried
5. customevaporated to an oil
6. dissolutionThe oil is dissolved in 300 ml
7. additiontoluene, treated with 15 ml
8. customThe solvents are evaporated
9. dissolutionthe residue is dissolved three times in toluene
10. customevaporating each time
11. customto yield a viscous, orange oil