ChemicalBook CAS DataBase List di-(tert-butyl)2-(2,2-diMethyl-4H-1,3-benzodioxin-6-yl)-2-oxoethyliMinodicarbonate

di-(tert-butyl)2-(2,2-diMethyl-4H-1,3-benzodioxin-6-yl)-2-oxoethyliMinodicarbonate synthesis

5synthesis methods

Product Name:di-(tert-butyl)2-(2,2-diMethyl-4H-1,3-benzodioxin-6-yl)-2-oxoethyliMinodicarbonate
CAS Number:452339-70-7
Molecular formula:C22H31NO7
Molecular Weight:421.48

51779-32-9 Synthesis

51779-32-9
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102293-80-1 Synthesis

2-Bromo-1-(2,2-dimethyl-4H-benzo[d][1,3]dioxin-6-yl)ethanone

102293-80-1
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di-(tert-butyl)2-(2,2-diMethyl-4H-1,3-benzodioxin-6-yl)-2-oxoethyliMinodicarbonate

452339-70-7
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Yield:452339-70-7 64%

Reaction Conditions:

with Cs₂CO₃ in acetonitrile at 20 - 25; for 6 h;Inert atmosphere;

Steps:

4 Preparation of Di(tert-butyl) 2-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-2-oxo ethylimido dicarbonate (VI)

Example 4
Preparation of Di(tert-butyl) 2-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-2-oxo ethylimido dicarbonate (VI)
Compound V (1.0 eqt), di-t-butyl imidino dicarboxylate (1.0 eqt) and cesium carbonate (1.2 eqt) were mixed together at 20-25° C. in acetonitrile under nitrogen over a period of 6 hr.
After completion of reaction, the reaction mass was filtered off and washed with acetonitrile and concentrated under vacuum below 50° C.
The residue thus obtained was dissolved in toluene and washed with water followed by brine.
The organic fractions were dried over anhydrous sodium sulfate and were concentrated under vacuum below 60° C. to obtain the crude product.
The crude compound was slurried with diisopropyl ether, filtered and dried under vacuum at 40-45° C. to obtain the tilted compound.
Yield: 64%; purity by HPLC: 99.57%

References:

US2015/239862,2015,A1 Location in patent:Paragraph 0127; 0128