Methyl 4-bromobenzoate → Methyl 4-[(3,5-difluorophenyl)methylamino]benzoate

HRID 483

반응식

HRID 483 반응식
COC(=O)c1ccc(Br)cc1.NCc1cc(F)cc(F)c1>CC(=O)O.CC(=O)O.Cc1ccccc1.O=C([O-])[O-].[Cs+].[Cs+].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>COC(=O)c1ccc(NCc2cc(F)cc(F)c2)cc1

참가 물질

7

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온도
100 °C

실험 절차

methyl 4-bromobenzoate (1.8 g, 8.37 mmol), (3,5-difluorophenyl)methanamine (1.980 mL, 16.74 mmol) and Cesium carbonate (2.73 g, 8.37 mmol) were mixed in toluene (4 mL) and degassed by bubbling nitrogen through solution. Palladium acetate (0.094 g, 0.42 mmol) and rac-2,2'-Bis(diphenylphosphino)-1,1'-binaphthyl (0.365 g, 0.59 mmol) were added and the vial was capped and heated at 100°C over 5 days. Workup by dilution with EtOAc, washing with water, then extraction with 2M HCl. The HCl extract was neutralized with 2M NaOH and extracted with EtOAc and the EtOAc phase was dried (K2CO3) and evaporated to give the crude product. The desired amine was not the compound isolated. Discarded.

출처 및 근거

ORD 기록
ord-a50a848eea9042a19d3b9efbefd39662
출처 데이터셋
750 AstraZeneca ELN dataset
원본 링크
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