反应 #417988

反应方程式

2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl

methylpiperazine

potassium phosphate trihydrate

2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl

3-[3-(5-iodopyrimidin-2-yl)benzyl]-5-trifluoromethyl-3H-benzothiazol-2-one

→

3-{3-[5-(4-methylpiperazin-1-yl)pyrimidin-2-yl]benzyl}-5-trifluoromethyl-3H-benzothiazol-2-one

溶剂

toluene

Water

反应条件

后处理

1. 1
   温度cooled to room temperature
2. 2
   workup.STIRRINGstirred at 100° C. for a further 24 h under an argon atmosphere
3. 3
   萃取is then extracted with ethyl acetate
4. 4
   其他dried
5. 5
   其他The crude product is purified by means of preparative HPLC

实验过程

513 mg (1 mmol) of 3-[3-(5-iodopyrimidin-2-yl)benzyl]-5-trifluoromethyl-3H-benzothiazol-2-one is suspended in toluene, briefly heated to 100° C. and cooled to room temperature. 134 μl (1.2 mmol) of methylpiperazine, 297 mg (1.4 mmol) of potassium phosphate trihydrate, and 33 mg (0.08 mmol) of 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl and 18 mg (0.02 mmol) of tris(benzylideneacetone)dipalladium are subsequently added and stirred at 100° C. under an argon atmosphere. 33 mg (0.08 mmol) of 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl and 18 mg (0.02 mmol) of tris(benzylideneacetone)dipalladium are subsequently again added and stirred at 100° C. for a further 24 h under an argon atmosphere. Water is added to the reaction mixture, which is then extracted with ethyl acetate and dried. The crude product is purified by means of preparative HPLC. The product is in the form of the trifluoroacetate.

来源