تفاعل #69032

معادلة التفاعل

(1-ethoxycyclopropoxy)trimethylsilane

acetic acid

1-(3-bromo-5-fluorophenyl)piperazine

→

1-(3-bromo-5-fluorophenyl)-4-cyclopropylpiperazine

المذيبات

THF

EtOAc

MeOH

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe resulting mixture was heated to 70 C overnight
2. 2
   تركيزconcentrated in vacuuo
3. 3
   أخرىto give crude residue which
4. 4
   غسيلwashed with 1 N NaOH
5. 5
   أخرىThe organic layer was separated
6. 6
   تجفيفdried with anhydrous MgSO4
7. 7
   ترشيحfiltered
8. 8
   تركيزconcentrated in vacuo

الإجراء التجريبي

To mixture of 1-(3-bromo-5-fluorophenyl)piperazine (2.91 g, 11 mmol) in MeOH (50 mL) was added (1-ethoxycyclopropoxy)trimethylsilane (13.5 mL, 67.2 mmol), acetic acid (6.5 mL, 112 mmol) and NaBCNH4 (1.0 M in THF) (51 mL, 50.4 mmol). The resulting mixture was heated to 70 C overnight and concentrated in vacuuo to give crude residue which was diluted with EtOAc and washed with 1 N NaOH followed by brine. The organic layer was separated, dried with anhydrous MgSO4, filtered and concentrated in vacuo to give desired 1-(3-bromo-5-fluorophenyl)-4-cyclopropylpiperazine in quantitative yield.

المصدر