反应 #1606839
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08946429B2
反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: (1-Bromo-2,2-dimethyl-propyl)-benzene (1.00 g, 4.40 mmol) was dissolved in dry DMF (5 mL) under an argon atmosphere. Potassium thioacetate (2.51 g, 22.0 mmol) was added and the reaction was heated to 50° C. for 7 days. The solution was then concentrated and the product purified by column chromatography to obtain the desired thioester (970 mg, 99%). TLC (Hexane:CH2Cl2, 7:3 v/v): Rf=0.40. 1H NMR (400 MHz, CDCl3): δ 7.33-7.22 (m, 5H), 4.52 (s, 1H), 2.32 (s, 3H), 1.00 (s, 9H). 13C NMR (100 MHz, CDCl3): δ 193.9 (q), 140.4 (q), 129.0, 127.2, 126.4, 58.7, 34.9 (q), 30.2, 27.6. HRMS (m/z): [M+Na]+ calcd. for C13H18ONaS 245.0976; found, 245.0972. The solution was then concentrated the product purified by column chromatography
来源 ID: ord-75eafea52e424fd195bda8cfc61eaa40