反応 #161710

反応方程式

sodium hydrogen carbonate

benzyl-(2,2,2-trifluorethyl)-amine

sodium hydroxide

6-chloropyrimidine-4-carboxylic acid chloride

→

6-chloropyrimidine-4-carboxylic acid-benzyl-(2,2,2-trifluoro-ethyl)-amide

溶媒

dichloromethane

反応条件

後処理

1. 1
   温度while being cooled
2. 2
   workup.WAITfor a further 1 h at RT
3. 3
   workup.STIRRINGthe mixture was stirred for 10 min
4. 4
   その他The organic phase was separated off
5. 5
   洗浄washed with water (1×30 mL) and 1M hydrochloric acid (1×50 mL)
6. 6
   その他dried on sodium sulphate
7. 7
   ろ過filtered
8. 8
   その他evaporated down i
9. 9
   その他The product was reacted further without any further purification

実験手順

1.04 g (5.50 mmol) benzyl-(2,2,2-trifluorethyl)-amine and 5.50 mL (5.50 mmol) of a 1M sodium hydroxide solution were added dropwise while cooling with a bath of ice/ethanol to 1.00 g (5.65 mmol) 6-chloropyrimidine-4-carboxylic acid chloride in 20 mL dichloromethane. The mixture was first stirred for 2 h while being cooled and then for a further 1 h at RT. 50 mL of a saturated sodium hydrogen carbonate solution were added and the mixture was stirred for 10 min. The organic phase was separated off, washed with water (1×30 mL) and 1M hydrochloric acid (1×50 mL), dried on sodium sulphate, filtered and evaporated down i. vac. The product was reacted further without any further purification.

出典