تفاعل #48701

معادلة التفاعل

trifluoromethanesulphonic anhydride

2-fluoro-2-methylpropan-1-ol

2,6-lutidine

→

desired compound

المردود 70.0%

Trifluoromethanesulfonic acid 2-fluoro-2-methylpropyl ester

المردود 70.0%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىAdd water to quench
2. 2
   أخرىthe reaction
3. 3
   أخرىseparate the organic layer
4. 4
   استخلاصextract the aqueous layer with dichloromethane
5. 5
   تجفيفdry (magnesium sulfate)
6. 6
   ترشيحfilter
7. 7
   تركيزconcentrate
8. 8
   أخرىpurify
9. 9
   غسيل(silica gel chromatography, eluting with dichloromethane)

الإجراء التجريبي

Add trifluoromethanesulphonic anhydride (4.3 mL, 26.0 mmol) to a solution of 2-fluoro-2-methylpropan-1-ol (2.0 g, 21.7 mmol) and 2,6-lutidine (3.0 mL, 26.0 mmol) in dichloromethane (25 mL) at −78° C. Warm slowly to room temperature and stir at room temperature for 1 hour. Add water to quench the reaction, separate the organic layer and extract the aqueous layer with dichloromethane. Combine the organic layers, dry (magnesium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with dichloromethane), to give the desired compound as an oil (3.4 g, 70% yield).

المصدر