反応 #329008

反応方程式

5-(4-Methyl-piperazin-1-ylmethyl)-2,3-dihydro-1H-isoindole

1,1′-Carbonyldiimidazole

2,4-bis-benzyloxy-5-isopropenyl-benzoic acid

→

title compound

収率 77.0%

(2,4-Bis-benzyloxy-5-isopropenyl-phenyl)-[5-(4-methyl-piperazin-1-ylmethyl)-1,3-dihydro-isoindol-2-yl]-methanone

収率 77.0%

溶媒

DMF

DMF

反応条件

後処理

1. 1
   その他The solid which had formed
2. 2
   その他was removed by filtration
3. 3
   洗浄washed with isopropyl acetate (2×21.6 L)
4. 4
   その他dried at 35° C. to constant weight

実験手順

1,1′-Carbonyldiimidazole (4.82 Kg, 29.8 mol) was added to a solution of 2,4-bis-benzyloxy-5-isopropenyl-benzoic acid (10.58 Kg, 28.3 mol, step 5) in DMF (21.2 L) at 25° C. After 20 mins at 25° C. a solution of 5-(4-Methyl-piperazin-1-ylmethyl)-2,3-dihydro-1H-isoindole (7.2 Kg, 31.1 mol, step 10) in DMF (7.2 L) maintaining a temperature below 35° C. and the solution stirred at 25° C. for a minimum of 12 h. The solid which had formed was removed by filtration, washed with isopropyl acetate (2×21.6 L) and dried at 35° C. to constant weight to give the title compound 8.7 Kg (77% yield, purity by hplc 97.5%).

出典