반응 #431102

반응 방정식

hexane ethanol

TFA

TFA

(±)cis-1-(3,4-dichlorobenzyl)-2-aminoindane

→

(±)cis-1-(3,4-Dichlorobenzyl)-2-methylaminoindane

용매

acetonitrile

water

반응 조건

후처리

1. 1
   온도Eluent composition increased linearly from 5%B to 80% B over 40min.

실험 절차

(±)cis-1-(3,4-Dichlorobenzyl)-2-methylaminoindane (7.49 g) was prepared from (±)cis-1-(3,4-dichlorobenzyl)-2-aminoindane (Preparation 2, Method B, 13.95 g) as described in Preparations 3-5 , and then converted into the single enantiomers (+)cis-1-(3,4-dichlorobenzyl)-2-methylaminoindane hydrochloride(E1) and (-)cis-1-(3,4-dichlorobenzyl)-2-methylaminoindane hydrochloride(E2) as described above. In each case chiral purity was greater than 99.5% as judged by chiral HPLC analysis (Column: CHIRALPAK AD; Eluent: 99/1 hexane/ethanol+0.1% DEA). The level of other impurities was<0.3% as judged by HPLC (Column: Merck RP--Select B. Eluent A: 0.1% TFA in water; Eluent B 0.1% TFA in acetonitrile; Eluent composition increased linearly from 5%B to 80% B over 40min. and then held at 80% B for a further 10 min).

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