Phosphorus oxychloride → HCID 10066297, compound

TEA (7.12 g, 70 mmol) was added dropwise to a stirred solution of bis(2-bromoethyl)amine hydrobromide (10.00 g, 32 mmol) and phosphorus oxychloride (4.91 g, 32 mmol) in CH2Cl2 (50 ml) at 0° C. under N2. The mixture was allowed to stir overnight and then poured over ice. The layers were separated, and the aqueous layer was extracted with CH2Cl2 (3×50 ml). The organic layers were combined and dried (MgSO4). The filtrate was concentrated under reduced pressure and the residue purified by chromatography (1:4 EtOAc: hexanes) to give 29 as an oil (3.86 g, 35%); 1H NMR (CDCl3) 3.70 (t, 4H, 6.73 Hz), 3.55 (t, 4H, 6.75 Hz)ppm.

1. additionpoured over ice
2. customThe layers were separated
3. extractionthe aqueous layer was extracted with CH2Cl2 (3×50 ml)
4. dry with materialdried (MgSO4)
5. concentrationThe filtrate was concentrated under reduced pressure
6. customthe residue purified by chromatography (1:4 EtOAc: hexanes)

ORD record

ord-3b425d9b3c96460892ac0f343e17f68e

Source dataset

uspto-grants-1993_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05233031