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68594-06-9

N-(Trifluoroacetyl)-1-desMethyl Daunorubicin synthesis

4synthesis methods
-

Yield:68594-06-9 94 %

Reaction Conditions:

with tetra-(n-butyl)ammonium iodide;potassium iodide;magnesium chloride in tetrahydrofuran at 60;Molecular sieve;

Steps:

4-6 Example 4: preparation of intermediate 3

Dissolve 20 g of intermediate 2 in 500 ml of tetrahydrofuran. 6.6g of anhydrous magnesium chloride, 10g of tetrabutylammonium iodide, 4.6g of anhydrous potassium iodide and 20g of molecular sieve, the mixture was stirred at 60 °C for 2 hours, filtered to obtain filtrate, added to ice water and acidified to pH 2.5 with trifluoroacetic acid, then the mixture was extracted with 2x150ml dichloromethane, the organic layer was dried with anhydrous MgSO4, and then the solvent was distilled under reduced pressure to obtain 15.9g intermediate 3 with a yield of 94% and HPLC purity of 96.72%, as shown in Figure 3.

References:

CN115785168,2023,A Location in patent:Paragraph 0052-0061