Synthetic Route of 118753-70-1, A common heterocyclic compound, 118753-70-1, name is tert-Butyl bis(2-chloroethyl)carbamate, molecular formula is C9H17Cl2NO2, 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.
(4-Chloro-2-fluorophenyl)acetonitrile (2.3 g, 13.7 mmol, 1.0 equiv) was added to a suspension of NaH (2.1 g, 52.5 mmol, 3.8 equiv) in DMSO (20 mL) at 23 C. The resulting yellow suspension was stirred for 10 min and the color turned red-brown. Boc-N(CH2CH2Cl) (N,N-bis(2-chloroethyl)-t-butylcarbamate) (3.7 g, 15.3 mmol, 1.1 equiv) in DMSO (20 mL) was added to the reaction mixture (bubbling observed) and the resulting suspension was heated to 85 C. with stirring for an additional 1.5 hours. The reaction mixture was cooled to 23 C. then poured onto a 1:1 mixture of ethyl acetate and hexanes (300 mL). The organic fraction was washed with water (100 mL) and a saturated aqueous solution of NaCl (100 mL). The organic layer was dried over anhydrous sodium sulfate. The dried solution was then filtered and the filtrate was concentrated. The residue was purified by flash silica chromatography (0%-30% ethyl acetate in hexanes) to afford the bis-alkylation product 1,1-dimethylethyl 4-(4-chloro-2-fluorophenyl)-4-cyano-1-piperidinecarboxylate (1.9 g, 5.6 mmol, 38%) as a yellow crystalline solid. MS (ES) m/e 239 [M-Boc+H]+.
The synthetic route of 118753-70-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Eidam, Hilary Schenck; Haile, Pamela A.; Hughes, Terry Vincent; Sehon, Clark A.; US2008/318990; (2008); A1;,
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