Synthetic Route of 36805-97-7, A common heterocyclic compound, 36805-97-7, name is 1,1-Di-tert-butoxy-N,N-dimethylmethanamine, molecular formula is C11H25NO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Step 1: A suspension of 6-chloro-4-(isopropylamino)nicotinic acid (240 g, 1118 mmol) in toluene (1800 mL) in a 1 L round bottom flask was heated to 90 C. N,N-dimethylformamide di-tert-butyl acetal (1609 mL, 6709 mmol) in toluene (1800 mL) was added slowly over 8-9 hrs. The reaction mixture was heated at 90 C. for 12 hrs. After completion of 12 hrs, the reaction mixture was cooled and concentrated under reduced pressure to remove excess of solvent and obtain the crude material. The crude material was purified by flash column chromatography using silica gel as stationary phase and EtOAc: pet ether (2:8) as eluent to afford the title compound, tert-butyl 6-chloro-4-(isopropylamino)nicotinate (275 g, 91% yield). LC/MS 271.0 (M+H). 1H NMR (400 MHz, CDCl3) delta=8.59 (s, 1H), 8.14-8.08 (m, 1H), 6.51 (s, 1H), 3.71-3.61 (m, 1H), 1.57 (s, 9H), 1.28 (d, J=6.5 Hz, 6H).
The synthetic route of 36805-97-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Santella, Joseph B.; Kumar, Sreekantha Ratna; Duncia, John V.; Gardner, Daniel S.; Paidi, Venkatram Reddy; Nair, Satheesh Kesavan; Hynes, John; Wu, Hong; Murugesan, Natesan; Sarkunam, Kandhasamy; Arunachalam, Piramanayagam; US2015/191464; (2015); A1;,
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