反応 #9200

反応方程式

N-methylmorpholine

1-ethyl-5-methyl-3-(6-nitro-1,3-benzothiazol-2-yl)-1,3,5-triazinan-2-one

N-Ethyl-N′-(6-nitro-1,3-benzothiazol-2-yl)urea

formaldehyde

MeNH2

→

title product

N-(6-Cyano-1,3-benzothiazol-2-yl)-N′-(3-pyridylmethyl)urea

溶媒

EtOH H2O

MeOH

反応条件

後処理

1. 1
   温度The slurry is then cooled to room temperature
2. 2
   ろ過filtered
3. 3
   洗浄washed well with water
4. 4
   その他dried

実験手順

General procedure for synthesizing 1-ethyl-5-methyl-3-(6-nitro-1,3-benzothiazol-2-yl)-1,3,5-triazinan-2-one: N-Ethyl-N′-(6-nitro-1,3-benzothiazol-2-yl)urea is suspended in an alkanol/water mixture, preferably 1:1 EtOH/H2O at room temperature. A 37% aqueous solution of formaldehyde is added followed by addition of a 2M solution of MeNH2 in MeOH, then about 2 mole equivalents of N-methylmorpholine. The solution is warmed to about 70–85° C., preferably 80° C., then allowed to stir for about 4–24 hours, preferably 4 hours. The slurry is then cooled to room temperature, filtered and washed well with water, dried and the title product is isolated. General Procedure for Grignard Addition:

出典