反应 #1911568
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09365576B2
反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 1,3-dimethyl-5-triisopropylsilanyloxy-tetrahydro-pyrimidin-2-one (Step P8) (9.1 g, 28 mmol) in EtOH (70 mL) was added a 1M HCl (140 mL, 140 mmol) and the mixture was stirred for 3 h at 70° C. The mixture was concentrated, and the pH of the resulting aqueous phase was adjusted to 5 with a saturated aqueous NaHCO3 solution. The aqueous layer was saturated with NaCl and was extracted with CH2Cl2/isopropanol 3:1. The organic layer was dried (Na2SO4), filtered and concentrated to afford the title compound. ESI-MS: tR=0.33 min, [M+H]+ 145.1 (LC-MS 1). The mixture was concentrated was extracted with CH2Cl2/isopropanol 3:1 The organic layer was dried (Na2SO4) filtered concentrated
来源 ID: ord-23ad60b1c589492e9eef7f5f279e4ade