Reference of 16066-84-5, A common heterocyclic compound, 16066-84-5, name is tert-Butyl methylcarbamate, molecular formula is C6H13NO2, 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 Preparation of Compound c71 (0551) Compound c70 (1.0g, 4.15mmol) was dissolved in dioxane (16mL), and tertiary butyl methyl carbamate (653mg, 4.98mmol), 2- dicyclohexylphosphino-2 ‘, 4′ , 6’-triisopropyl-biphenyl (297mg, 0.622mmol), potassium phosphate (2.20g, 10.73mmol) and tris (dibenzylideneacetone) palladium (190mg, 0.207mmol) were added to the mixture at 100 C for 5 hours. Tertiary butyl methyl carbamate (218mg, 1.66mmol), 2-dicyclohexylphosphino-2 ‘, 4′, 6’-triisopropyl biphenyl (99mg, 0.207mmol), potassium phosphate (0.73g, 3.57mmol) and tris (dibenzylideneacetone) palladium (0) (63.3mg, 0.069mmol) were added to the mixture and the mixture was stirred for 3 hours. Tertiary butyl methyl carbamate (435mg, 3.32mmol), 2- dicyclohexylphosphino-2 ‘, 4′, 6’-triisopropyl biphenyl (99mg, 0.207mmol) and tris (dibenzylideneacetone) palladium (0) (63.3mg, 0.069mmol) was then added to the mixture and the mixture was stirred for 5.5 hours. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate) to give compound c71 (0.75g, 74% yield). [M + H] = 244.95, Method Condition 3: retention time 2.08 min
The synthetic route of 16066-84-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Shionogi & Co., Ltd.; KOBAYASHI, Naotake; ASAHI, Kentarou; TOMIDA, Yutaka; OHDAN, Masahide; FUMOTO, Masataka; SASAKI, Yoshikazu; KURAHASHI, Kana; INOUE, Takatsugu; URABE, Tomomi; NISHIURA, Yuji; IWATSU, Masafumi; MIYAZAKI, Keisuke; OHYABU, Naoki; WADA, Toshihiro; KATOU, Manabu; (276 pag.)EP3059225; (2016); A1;,
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