ChemicalBook CAS DataBase List 2-Oxazolidinone, 5-(2,2-diMethyl-4H-1,3-benzodioxin-6-yl)-, (5R)-

2-Oxazolidinone, 5-(2,2-diMethyl-4H-1,3-benzodioxin-6-yl)-, (5R)- synthesis

8synthesis methods

Product Name:2-Oxazolidinone, 5-(2,2-diMethyl-4H-1,3-benzodioxin-6-yl)-, (5R)-
CAS Number:452339-73-0
Molecular formula:C13H15NO4
Molecular Weight:249.26

(R)-2-amino-1-(2,2-dimethyl-4H-benzo[d][1,3]dioxin-6-yl)ethan-1-ol (29.8g, 134.0mmol, 1.0eq.) and tetrahydrofuran (300mL) were added to the reaction flask under nitrogen protection, the reaction solution was heated to 40-60°C, and N, N'- Carbonyldiimidazole (22.7 g, 140.0 mmol, 1.05 eq.).After the addition, the reaction solution was kept at a temperature of 40-60° C. and stirred until the raw material reaction was completed. After the reaction, the solution was cooled to 15-30° C., and water (400 mL) was added. Then, the mixture was continuously cooled to 0-10°C and kept stirring. The precipitated solid was filtered, and the filter cake was washed with water. The filter cake was collected and dried under reduced pressure to obtain 2-Oxazolidinone, 5-(2,2-diMethyl-4H-1,3-benzodioxin-6-yl)-, (5R)- (30 g, 120.4 mmol, 89.9% yield).

2-Oxazolidinone, 5-(2,2-diMethyl-4H-1,3-benzodioxin-6-yl)-, (5R)-

452339-72-9 Synthesis

CarbaMic acid, [(2R)-2-(2,2-diMethyl-4H-1,3-benzodioxin-6-yl)-2-hydroxyethyl]-, 1,1-diMethylethyl ester

452339-72-9
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452339-73-0
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Yield:452339-73-0 90.2%

Reaction Conditions:

with heteropoly acid in ethyl acetate at 10 - 15;Solvent;Temperature;

Steps:

1.2 Second, the catalytic preparation of verapamil triphenylacetate intermediate, namely (II) compounds, the reaction equation is as follows:

Take (1) 5g of raw materials was added to 40ml of ethyl acetate was stirred, then add 0.05 heteropoly acid crystals 10-15 ° C reaction3-5h, HPLC detection of the reaction solution, when (1) the type of raw material no longer down to stop the reaction, cooled to room temperature; using a pore size of 0.2 micronsMicroporous membrane filter to remove heteropoly acid crystals, washed, concentrated to give the product.

References:

CN106957313,2017,A Location in patent:Paragraph 0014-0015

102293-80-1 Synthesis