반응 #161710
ord-85f255f912d74627b1b16b998fbcf446
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도while being cooled
- 2workup.WAITfor a further 1 h at RT
- 3workup.STIRRINGthe mixture was stirred for 10 min
- 4기타The organic phase was separated off
- 5세척washed with water (1×30 mL) and 1M hydrochloric acid (1×50 mL)
- 6기타dried on sodium sulphate
- 7여과filtered
- 8기타evaporated down i
- 9기타The product was reacted further without any further purification
실험 절차
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.