In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 110661-91-1 as follows. Application In Synthesis of tert-Butyl 4-bromobutanoate
To a mechanically stirred solution of terf-butyl 4-bromobutanoate [CAS 1 10661 – 91 -1] (42.3 g, 0.19 mol) in DMF (600 mL) was added in portions a solid mixture of 3-amino-5-methoxyphenol [CAS 162155-27-3] (26.4 g, 0.19 mol) and Cs2CO3 (123.6 g, 0.379 mol). The reaction was stirred at 60C for 65 h, and allowed to reach room temperature. The mixture was poured out into H2O (2.5 L). The product was extracted with Et2O (2 times). The combined organic layers were washed with brine, dried over MgSO4 and filtered off. The solvent was evaporated under reduced pressure, and then co-evaporated with toluene. The residue was purified via Normal Phase HPLC (Stationary phase: silica gel 60A 25-40 muiotatauiota (Merck), Mobile phase: gradient from 20% EtOAc, 80% heptane to 60% EtOAc, 40% heptane) yielding te/t-butyl 4-(3-amino-5-methoxyphenoxy)butanoate 1a (27 g).
According to the analysis of related databases, 110661-91-1, the application of this compound in the production field has become more and more popular.
Reference:
Patent; JANSSEN PHARMACEUTICALS, INC.; KATHOLIEKE UNIVERSITEIT LEUVEN; KESTELEYN, Bart Rudolf Romanie; RABOISSON, Pierre Jean-Marie Bernard; BONFANTI, Jean-Francois; BARDIOT, Dorothee Alice Marie-Eve; MARCHAND, Arnaud Didier M; (74 pag.)WO2017/167951; (2017); A1;,
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