1,2-Ethanediamine, N,N-bis(2-chloroethyl)-, dihydrochloride → 3399-66-4

N,N-Bis(2-chloroethyl)ethylenediamine (DCE) A solution of the above diol (2.96 g, 0.02 mol) in SOCl2 (150 mL) was stirred at room temperature for 48 h. Excess SOCl2 was then removed under reduced pressure, and the residue was dissolved in water and washed several times with EtOAc. The aqueous layer was evaporated to dryness under reduced pressure, and the resulting crude residue was crystallised from MeOH to give N,N-bis-(2-chloroethyl)ethylenediamine dihydrochloride (DCE.2HCl) as hygroscopic white plates, mp 136° C. (Price, Kavas and Nakata, J. Med. Chem., 1965, 8, 650, record mp 139°-140° C.).

1. customExcess SOCl2 was then removed under reduced pressure
2. dissolutionthe residue was dissolved in water
3. washwashed several times with EtOAc
4. customThe aqueous layer was evaporated to dryness under reduced pressure
5. customthe resulting crude residue was crystallised from MeOH

ORDレコード

ord-b67805370fff4684bb7faa4d21ee8cc8

出典データセット

uspto-grants-1996_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05554648