As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. COA of Formula: C5H12O2
5t (1.0 mmol), carbodiimide (CDI, 1.1 mmol), and DMAP(0.1 mmol) were sequentially added under air to a reaction tubeequipped with a stir bar and a septum. Et3N (1.5 mmol) and CH2Cl2(2 mL) was added by syringe and the resulting mixture vigorouslystirred for 3 h at ambient temperature. After this time, 8i(2.0 mmol) was sequentially added to this solution and the result-ing mixture again stirred for 14 h at ambient temperature. After thistime, the resulting solution was quenched with sat. NH4Claq andextracted with EtOAc. The solution obtained was ltered throughthe plug of silica gel and anhydrous MgSO4, and then concentratedby rotary evaporation. The pure product 9i was obtained byrecrystallization (65%, X mg, X mmol). IR(neat): 3484, 3341, 2970,1684, 1594, 1515, 1272, 1102 cm1.1H NMR (500 MHz, CDCl3) d: 8.59(brs, 1H), 8.02 (d, J 8.7 Hz, 2H), 7.63 (d, J 8.7 Hz, 2H), 4.49 (t,J 6.8 Hz, 2H), 2.05 (s, 6H), 1.98 (t, J 6.8 Hz, 2H), 1.32 (s, 6H);13CNMR (125 MHz, CDCl3) d: 170.30, 166.13, 141.66, 130.81, 126.32,119.23, 70.05, 62.49, 62.07, 41.80, 32.42, 29.81. HRESIMS calcd. forC16H23O4NBr (MH): 372.0810; found 372.0811.
With the rapid development of chemical substances, we look forward to future research findings about 2568-33-4.
Reference:
Article; Murata, Yumi; Takeuchi, Kentaro; Nishikata, Takashi; Tetrahedron; vol. 75; 18; (2019); p. 2726 – 2736;,
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