反应 #3039965
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09226930B2
反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of D10 (1.083 g, 3.955 mmol), 2,2-dimethyl-1-phenylpiperazine (0.903 g, 4.745 mmol) [C.A.S. 2946-75-0] and DIPEA (1.378 ml, 7.909 mmol) in CH3CN (15 ml) was heated in a sealed tube at 100° C. for 5 days. After cooling, the solvent was concentrated in vacuo. The residue was purified by column chromatography (silica gel; Heptane/EtOAc 100/10 to 80/20 as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate D55 (0.56 g, 42%). After cooling the solvent was concentrated in vacuo The residue was purified by column chromatography (silica gel; Heptane/EtOAc 100/10 to 80/20 as eluent) The desired fractions were collected concentrated in vacuo to yield intermediate D55 (0.56 g, 42%)
来源 ID: ord-e4239f840bdb48a38cc4f6e2bf399aa1