6,9,12-Trioxa-2,16-diazaoctadecanoic acid, 18-chloro-17-oxo-, 1,1-dimethylethyl ester synthesis
- Product Name:6,9,12-Trioxa-2,16-diazaoctadecanoic acid, 18-chloro-17-oxo-, 1,1-dimethylethyl ester
- CAS Number:934164-55-3
- Molecular formula:C17H33ClN2O6
- Molecular Weight:396.91
79-04-9
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194920-62-2
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934164-55-3
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Yield:934164-55-3 90%
Reaction Conditions:
with potassium carbonate in dichloromethane;water monomer;acetone;
Steps:
24 2
Tert-butyl 16-chloro-15-oxo-4,7,10-trioxa-14-azahexadec-1-ylcarbamate 10 g of tert-butyl 3-{2-[2-(3-aminopropoxy)ethoxy]ethoxy}propyl-carbamate is dissolved in 50 ml of CH2Cl2, in a three-necked flask equipped with a bath of acetone and ice. 5 g of K2CO3 dissolved in 50 ml of water and 5 g of chloroacetyl chloride dissolved in 50 ml of CH2Cl2 are added dropwise and simultaneously, by means of a dropping funnel. During the addition, the temperature of the medium is maintained at 0° C. When all the reagents have been added, the reaction medium is maintained with magnetic stirring, at ambient temperature for 1 hour. The 2 phases obtained are separated and the chloromethylene phase is then washed with water until neutral pH, dried over Na2SO4, filtered, and then concentrated. 11.2 g of product are obtained with a yield of 90%. Mass spectrum: M/z=397.4 (ES +) theoretical M=396.9
References:
US2010/297025,2010,A1
4246-51-9
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934164-55-3
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34619-03-9
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934164-55-3
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