Related Products of 35180-01-9, A common heterocyclic compound, 35180-01-9, name is Chloromethyl isopropyl carbonate, molecular formula is C5H9ClO3, 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 1Process for the Preparation of Tenofovir Disoproxil FumarateToluene (500 ml) was added to the Tenofovir (100 gm) and stirred at room temperature. To this triethylamine (66.31 gm) was added, temperature was raised to 90 C. and water was collected by azeotropic distillation at 110 C. Toluene was completely distilled under vacuum at same temperature. The reaction mixture was cooled to room temperature and to this a mixture of N-methyl pyrrolidine (300 gm), triethylamine (66.31 gm), Tetrabutyl ammonium bromide (52.8 gm) and trimethyl silyl chloride (17.8 gm) were added. The above reaction mixture was heated to 50-55 C. and was added slowly chloromethyl isopropyl carbonate (CMIC) and maintained the reaction mixture at 50-55 C. for 5 hrs. (Qualitative HPLC analysis shows about 85% product formation). The above reaction mixture was cooled to room temperature and filtered. The filtrate was added to DM water at 5-10 C. and extract with dichloromethane. The combined dichloromethane layer was concentrated under vacuum and the crude was Co-distilled with cyclohexane and this crude was taken into isopropyl alcohol (1000 ml). To this fumaric acid (38 gm) was added and temperature was raised to 50 C. The reaction mixture was filtered and filtrate was cooled to 5-10 C. The obtained solid was filtered and washed with isopropyl alcohol. The compound was dried under vacuum to yield Tenofovir Disoproxil fumarate (140 gm).
The synthetic route of 35180-01-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Datta, Debashish; Vellanki, Siva Rama Prasad; Sahu, Arabinda; Balusu, Raja Babu; Ravi, Mastan Rao; Nandipati, Hari Babu; Rama, Shankar; Vadali, Lakshmana Rao; Gorantla, Srikanth Sarat Chandra; Dasari, Srinivasa Rao; Mittapelly, Nagaraju; US2013/5969; (2013); A1;,
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