Реакция #48541

Уравнение реакции

30

3-fluoro-5-difluoromethyl-1-bromo-benzene

potassium t-butoxide

THF

NaHCO3

→

32

1-bromo-3-difluoromethyl-5-(4-methoxy-benzyloxy)-benzene

Растворители

Toluene

water

Условия реакции

Обработка

1. 1
   workup.STIRRINGAfter stirring at 65° C. for 2 h
2. 2
   ТемператураAfter cooling to RT
3. 3
   workup.ADDITIONwas added
4. 4
   Другоеthe organic phase separated
5. 5
   Промывкаwashed with a mixture of saturated NaHCO3 solution (75 mL) and water (75 mL)
6. 6
   ФильтрацияPolish filtration and concentration in vacuo

Методика

steps 3-5—p-Methoxybenzyl alcohol (36.8 g, 266.7 mmol) was added slowly to a mixture of potassium t-butoxide (28.7 g, 255.5 mol) and THF (250 mL). After stirring for about 15 min, 30 (50.0 g, 222.2 mmol) was added and the reaction mixture heated to about 65° C. After stirring at 65° C. for 2 h, the reaction is analyzed by HPLC. After cooling to RT, a mixture of saturated NaHCO3 solution (150 mL) and water (150 mL) was added. Toluene (300 mL) was added, the organic phase separated and washed with a mixture of saturated NaHCO3 solution (75 mL) and water (75 mL). Polish filtration and concentration in vacuo provided 83.9 g of crude 32 as an oil which is used without further purification.

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