Bromobenzene → 1,2-Diphenylpiperidine

HRID 569

반응식

HRID 569 반응식
Brc1ccccc1.c1ccc(C2CCCCN2)cc1>C1COCCO1.CC(C)Oc1cccc(OC(C)C)c1-c1ccccc1P(C1CCCCC1)C1CCCCC1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C([O-])[O-].[Cs+].[Cs+].[Pd].[Pd]>c1ccc(C2CCCCN2c2ccccc2)cc1

참가 물질

7

반응 조건

온도
100 °C

실험 절차

Caesium carbonate (556 mg, 1.71 mmol) was added to bromobenzene (0.060 mL, 0.57 mmol) and 2-phenylpiperidine (110 mg, 0.68 mmol) in 1,4-dioxane (2 mL). The reaction was degassed and Tris(dibenzylideneacetone)?dipalladium(0) (13.01 mg, 0.01 mmol) and dicyclohexyl(2',6'-diisopropoxy-[1,1'-biphenyl]-2-yl)phosphine (RuPhos) (13.26 mg, 0.03 mmol) were added. The resulting solution was stirred at 100 °C for 16 hours. LCMS showed The reaction mixture was diluted with EtOAc, and washed with water. The organic layer was dried over MgSO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 0 to 15% MeOH in DCM. Pure fractions were evaporated to dryness to afford 1,2-diphenylpiperidine (21.00 mg, 15.56 %) as a yellow oil. f0 = 19 mg bromobenzene f1 = 21 mg product The reaction was abandonned.

출처 및 근거

ORD 기록
ord-bd4700a79525457dbcfd3c5e1368118f
출처 데이터셋
750 AstraZeneca ELN dataset
원본 링크
출처 보기

연결된 노트

불러오는 중…