Cesium carbonate → Tert-butyl 4-(4-chloro-2-methylphenyl)piperazine-1-carboxylate

온도

80 °C

2-Bromo-5-chlorotoluene (0.82 g, 4 mmol) and tert-Butyl 1-piperazine carboxylate (0.89 g, 2.32 mmol) were added to a solution of tri-t-butyl phosphine (0.033 g, 4 mmol %), tris(dibenzylideneacetone)dipalladium(0) (0.075 g, 2.0 mmol %) and cesium carbonate (1.95 g, 6.0 mmol) in toluene and heated to 80° C. overnight. The reaction mixture was filtered through celite and concentrated in vacuo. The crude product was purified on silica gel (gradient elution from 20% ethyl acetate/hexane to 50% ethyl acetate/hexane) to give the title compound in 20% yield. ESI-MS m/z: 311 (M+1), UV retention time: 3.49 min.

1. filtrationThe reaction mixture was filtered through celite and
2. concentrationconcentrated in vacuo
3. customThe crude product was purified on silica gel (gradient elution from 20% ethyl acetate/hexane to 50% ethyl acetate/hexane)

ORD 기록

ord-6b5c1f8277504c4689871d4a49871d23

출처 데이터셋

uspto-grants-2007_03

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07186729B2