Electric Literature of 24310-36-9, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 24310-36-9 as follows.
Step 5. Preparation of 1, 2,3, 4-Tetrahydro-benzo [b] azepin-5-one. To preheated polyphosphoric acid (PPA, 220 g) at 70-80 C was added 1- (Toluene-4-sulfonyl)-1, 2,3, 4-tetrahydro-benzo [b] azepin-5-one (50.0 g, 0.16 mol). The mixture was stirred for 3.0 h at the same temperature and then poured into ice water. After the pH was adjusted to about 8-9 by adding aq NaOH, the mixture was extracted with ethyl acetate. The organic layer was separated, dried over MgS04, and concentrated. The residue was purified by silica gel column chromatography (eluent, 3: 1 n-hexanes: ethyl acetate) to give 1, 2,3, 4-Tetrahydro-benzo [b] azepin-5-one (22g).
According to the analysis of related databases, 24310-36-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ELI LILLY AND COMPANY; WO2005/37796; (2005); A1;,
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