反应 #452466

反应方程式

N-(4-bromobenzyl)-N-(pyridin-2-yl)pro-pane-1,3-diamine

3-morpholinopropyl isothiocyanate

→

title compound

收率 76.0%

1-(3-(N-(4-Bromobenzyl)-N-(pyridin-2-yl)amino)propyl)-3-(3-(morpholin-4-yl)propyl)thiourea

收率 76.0%

溶剂

chloroform

反应条件

后处理

1. 1
   温度at reflux temperature
2. 2
   workup.STIRRINGthe reaction mixture was stirred for an additional 4 h
3. 3
   温度at reflux temperature
4. 4
   其他The volatiles were evaporated in vacuo
5. 5
   workup.DISSOLUTIONthe residue (2.05 g) was dissolved in ethyl acetate (20 ml)
6. 6
   workup.WAITleft over night at room temperature
7. 7
   过滤The precipitate was filtered off
8. 8
   洗涤washed with ethyl acetate
9. 9
   其他dried

实验过程

To a solution of N-(4-bromobenzyl)-N-(pyridin-2-yl)pro-pane-1,3-diamine (1.0 g, 3.123 mmol) in chloroform (40 ml) was added 3-morpholinopropyl isothiocyanate (593 mg, 3.123 mmol) and the reaction mixture was stirred for 20 h at reflux temperature. To the reaction mixture was added 10 drops of 3-morpholinopropyl isothiocyanate and the reaction mixture was stirred for an additional 4 h at reflux temperature. The volatiles were evaporated in vacuo and the residue (2.05 g) was dissolved in ethyl acetate (20 ml) and left over night at room temperature. The precipitate was filtered off and washed with ethyl acetate and dried affording 1.20 g (76%) of the title compound as a solid.

来源