反応 #366918

反応方程式

2-amino-4-methoxy-6-methyl-1,3,5-triazine

2-biphenylylsulfonyl isocyanate

→

N-2-biphenylylsulfonyl-N'-(4-methoxy-6-methyl-1,3,5-triazin-2-yl) urea

溶媒

xylene

acetonitrile

反応条件

後処理

1. 1
   workup.ADDITIONDuring this addition
2. 2
   温度cooling
3. 3
   workup.ADDITIONAfter the addition
4. 4
   workup.WAITat 40° C. for 5 hours
5. 5
   ろ過the precipitated colorless crystals were filtered
6. 6
   洗浄washed with ether
7. 7
   その他dried

実験手順

14.0 g of 2-amino-4-methoxy-6-methyl-1,3,5-triazine were suspended in 100 ml of dry acetonitrile, and then 0.1 g of 1,4-diazabicyclo[2,2,2]octane was added thereto. To this mixture was added dropwise a solution of 2.5 g of 2-biphenylylsulfonyl isocyanate in 30 ml of xylene over an hour. During this addition, the reaction was accompanied by slight heat generation, and therefore cooling was applied as necessary. After the addition, the reaction was continued at room temperature for 5 hours and then at 40° C. for 5 hours. After allowing the mixture to cool to room temperature, the precipitated colorless crystals were filtered, washed with ether and dried to obtain 33.9 g of N-2-biphenylylsulfonyl-N'-(4-methoxy-6-methyl-1,3,5-triazin-2-yl) urea; m.pt. 190°-193° C.

出典