反应详情

Chloroacetyl chloride (6.63 ml) and triethylamine (13.4 ml) in DCM (20 ml) was added dropwise to 1-ethylpiperazine (10 g) in DCM (60 ml) under nitrogen. The mixture was stirred at room temperature for 17 hours then partitioned between DCM and H2O (100 ml). The aqueous layer was neutralised using 1M NaOH before extracting into DCM. Organic layer dried (MgSO4) and concentrated in vacuo. Purification by column chromatography (silica, 0 to 5% MeOH in DCM) gave the title compound as a pale oil (3.23 g, 19%). δH (CDCl3) 4.08 (2H, s), 3.65 (2H, m), 3.55 (2H, m), 2.52-2.40 (6H, m), 1.10 (3H, t, J 7.2 Hz).

1. customthen partitioned between DCM and H2O (100 ml)
2. extractionbefore extracting into DCM
3. dry with materialOrganic layer dried (MgSO4)
4. concentrationconcentrated in vacuo
5. customPurification by column chromatography (silica, 0 to 5% MeOH in DCM)