Application of 35180-01-9, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 35180-01-9, name is Chloromethyl isopropyl carbonate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
Example 9 Preparation of Tenofovir Disoproxil Fumarate [0092] To a clean 3-necked 1 L round bottom flask equipped with a mechanical stirrer, thermometer socket, addition funnel and dean-stark apparatus was charged cyclohexane (400 ml) and tenofovir (50 gms, obtained from example 1) and triethyl amine (34 gms) at temperature 20 C. to 35 C. Heated to 80 C. to 85 C. and stirred for 2 hours and simultaneously removed water liberated. The solvent was removed completely from the reaction mixture by distillation under vacuum at below 65 C. and to the obtained residue N-methyl pyrrolidinone (150 ml) and triethyl amine (34 gms) were charged at 25 C. to 30 C. Heated to 50 C. to 55 C. and chloromethyl isopropyl carbonate (125 gms) was added at same temperature and stirred for 4 hours. After completion of the reaction, the reaction mass was cooled to 20 C. to 25 C. and washed with cyclohexane (200 ml). Methylene chloride (500 ml) was charged into the organic layer and stirred for 1 hour at 10 C. to 15 C. Filtered the salts formed and washed the filtrate with water (500 ml), separated the layers and charged water (500 ml) to the organic layer. Adjusted pH to 6.5 to 7.5 with 10% ammonia solution and separated the organic layer from the aqueous layer. The solvent was removed from the organic layer under vacuum at below 35 C. to obtain oily product and then the oily product was diluted with isopropanol (150 ml). [0093] In a clean another 3-necked 1 L round bottom flask equipped with a mechanical stirrer, thermometer socket and addition funnel was charged isopropanol (350 ml) and Fumaric acid (19 gms). Heated to 50 C. to 55 C. and stirred for 20 minutes and above obtained oily product solution was added at 50 C. to 55 C. Stirred for 30 minutes at this temperature and cooled to 0 C. to 5 C. Filtered the product and washed with chilled isopropanol (75 ml). The wet product was dried at 35 C. to 40 C. under reduced pressure to provide the title compound as crude (80 gms). [0094] In another clean 3-necked 1 L round bottom flask equipped with a mechanical stirrer, thermometer socket and addition funnel was charged ethyl acetate (450 ml) and crude product (80 gms) at temperature 10 C. to 15 C. Stirred the slurry for 1 hour and filtered the product and washed with chilled ethyl acetate (50 ml). The wet product was dried at 35 C. to 40 C. for 6 hours under reduced pressure to provide the title compound. [0095] Yield: 55 gms. [0096] HPLC purity: 98.9%
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Chloromethyl isopropyl carbonate, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; Laurus Labs Private Limited; Indukuri, Venkata Sunil Kumar; Joga, Sree Rambabu; Gorantla, Seeta Ramanjaneyulu; Chava, Satyanarayana; US2014/303368; (2014); A1;,
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