تفاعل #607446

معادلة التفاعل

2,2,2-trifluoro-1-[4-(trifluoromethyl)phenyl]ethanone

sodium borohydride

NH4Cl

→

2,2,2-trifluoro-1-[4-(trifluoromethyl)phenyl]ethanol

المردود 105.1%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooling
2. 2
   workup.STIRRINGwith additional stirring for 10 min
3. 3
   استخلاصThe later was extracted 3 times with 20 mL of EtOAc
4. 4
   غسيلwashed with 10 mL of brine
5. 5
   تجفيفdried over Na2SO4
6. 6
   ترشيحfiltered
7. 7
   أخرىThe solvent was removed under reduced pressure

الإجراء التجريبي

In a 50 mL two-neck flask, 2,2,2-trifluoro-1-[4-(trifluoromethyl)phenyl]ethanone (2.0 g, 8.3 mmol) was dissolved in methanol (8 mL) and sodium borohydride (0.31 g, 8.3 mmol) was added carefully in portions with ice-bath cooling. The resultant colourless solution was stirred at RT for 2 hours and monitored by TLC. Upon the disappearance of all starting material, 5 mL of an aqueous saturated NH4Cl solution was slowly added to the reaction mixture with additional stirring for 10 min. The later was extracted 3 times with 20 mL of EtOAc and the organic fractions were combined and washed with 10 mL of brine, dried over Na2SO4, and filtered. The solvent was removed under reduced pressure to give 2,2,2-trifluoro-1-[4-(trifluoromethyl)phenyl]ethanol (2.13 g, quantitative) as a colourless oil which was used with no further purification.

المصدر