Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 73790-19-9, name is 5-Bromo-2,2-dimethylbenzo[d][1,3]dioxole, A new synthetic method of this compound is introduced below., Safety of 5-Bromo-2,2-dimethylbenzo[d][1,3]dioxole
4-BROMO-1, 2-dihydroxybenzolacetonide A (160.0 g) was combined with NA2C03 (72.0 g), DPPE (12.7g), Pd (OAC) 2 (3.8 g) and acrolein ethylenacetal B (127.0 g) were suspended under an N2 atmosphere in DMF (200.0 g). The yellow suspension was heated to 105-110 C for 32-36 hours, at which time the suspension turned a brownish color. After 32-36 hours, an in process control (IPC) was performed, whereby if the amount of starting material less than 2% (HPLC), the suspension is cooled down to 25C and 320 g of ethyl acetate is added. If the amount of starting material is greater than 2%, the suspension is heated for two additional hours. The suspension was then filtered over nutsch and the residue rinsed with ethyl acetate (320.0 g). Water (640.0 g) and NaCl (19.2 g) were added and the mixture heated to 55-60 C for 10 min. The phases were then separated and the aqueous. phase was discarded. Water (334 g) and NACL (13.4 g) were added to the organic phase, the mixture was well agitated, and the phases were separated. The organic phase was then concentrated under vacuum to provide a brownish oil (208 g) which was used without further purification.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; LYMPHOSIGN INC.; WO2005/777; (2005); A2;,
Bromide – Wikipedia,
bromide – Wiktionary