반응 #69032

반응 방정식

(1-ethoxycyclopropoxy)trimethylsilane

acetic acid

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

→

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

용매

THF

EtOAc

MeOH

반응 조건

후처리

1. 1
   온도The resulting mixture was heated to 70 C overnight
2. 2
   농축concentrated in vacuuo
3. 3
   기타to give crude residue which
4. 4
   세척washed with 1 N NaOH
5. 5
   기타The organic layer was separated
6. 6
   건조dried with anhydrous MgSO4
7. 7
   여과filtered
8. 8
   농축concentrated in vacuo

실험 절차

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.

출처