CarbaMic acid, bis(2-chloroethyl)-, phenyl ester synthesis
- Product Name:CarbaMic acid, bis(2-chloroethyl)-, phenyl ester
- CAS Number:13249-63-3
- Molecular formula:C11H13Cl2NO2
- Molecular Weight:262.13
Yield:-
Reaction Conditions:
Stage #1: bis-(2-chloroethyl)amine hydrochloride;phenyl chloroformate in dichloromethane at 0; for 0.166667 h;
Stage #2: with triethylamine in dichloromethane at 20; for 1.33333 h;Product distribution / selectivity;
Steps:
2
5 g of Bis(2-chloroethyl)amine HCl was suspended in 30 ml of pre-dried dichloromethane. 4.7 g of phenylchloroformate was added with cooling (ice water) and stirring, while N2 was bubbled through the mixture. The addition was complete within 10 min and was followed by addition of 8.5 ml of triethylamine during 20 minutes.The mixture was further stirred at ambient temperature for 1 hour:Then, 10 ml of water was added, and the mixture was stirred for 50 min. till the solid dissolved. The organic layer was separated and washed with 10 ml of HCl 1M and 10 ml of saturated aqueous NaCl. The organic layer was dried and concentrated in vacuo to give an oily product (6.7 g).
References:
US2009/143582,2009,A1 Location in patent:Page/Page column 5
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