反应 #3450134
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09394276B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Intermediate 10A (2.6 g, 9.77 mmol) was deprotected with 30% TFA in DCM (40 mL). After 2 h, the reaction was concentrated and the residue was partitioned with EtOAc (75 mL) and saturated NaHCO3 (50 mL). The organic layer was washed with brine (20 mL) and dried (MgSO4). Crude Intermediate 10B was carried onto the next step. 1H NMR (400 MHz, DMSO-d6) δ 9.86 (1H, s), 7.56 (2H, d, J=8.84 Hz), 7.28 (2H, d, J=8.84 Hz), 6.90 (2H, s), 3.68 (3H, s) ppm. the reaction was concentrated the residue was partitioned with EtOAc (75 mL) and saturated NaHCO3 (50 mL) The organic layer was washed with brine (20 mL) dried (MgSO4)
来源 ID: ord-b2360a0323e748f787e7420d1f641269