Electric Literature of 22246-76-0, These common heterocyclic compound, 22246-76-0, name is 8-Amino-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one, 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.
Example No. 217Preparation of methyl 3- (7- ( (2-oxo-2 , 3 , 4 , 5-tetrahydro-lH- benzo [b] azepin-8-yl) amino) -IH-pyrazolo [4, 3-d] pyrimidin- 5- yl) benzoate methyl 3- (7-chloro-2- (4-methoxybenzyl) -2H-pyrazolo [4,3- d] pyrimidin- 5 -yl) benzoate (0.16 mmol) and 8 -amino-4 , 5 -dihydro- lH-benzo [b] azepin-2 (3H) -one (0.3 mmol 2 eq. , ) were suspended in MeOH (dry, 3mL) in a microwave vial (2-5mL) , HC1 in dioxane (4M, 3 drops) was added. The reaction mixture was irradiated in a microwave reactor for 5 min at 140C. The reaction mixture was evaporated and used without further purification. The residue was dissolved in TFA (3mL) . The reaction mixture was irradiated in a microwave reactor for 5 min at 140C. The reaction mixture was concentrated and purified by semi- preparative HPLC-MS and freeze dried from water/t-BuOH 4/1. exact mass: 428.1868 g/molHPLC-MS: analytical method Lrt: 4.65 min – found mass: 429 (m/z+H)
The synthetic route of 22246-76-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ORIGENIS GMBH; ALMSTETTER, Michael; THORMANN, Michael; TREML, Andreas; TRAUBE, Nadine; WO2012/143144; (2012); A1;,
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