1,2-Ethanediamine, N1,N1,N2-trimethyl- → HCID 21135479, compound

Under Ar, a solution of CH3OSi(CH3)2(CH2)3Cl (10.0 g, 59.3 mmol), CH3NHCH2CH2N(CH3)2 (10.0 g, 98.2 mmol) and methanol (5.0 mL) is refluxed for 22 h and then concentrated with a rotary evaporator (about 10 Torr, about 45 ° C.). The concentrate is diluted with ether (50 mL) and filtered. The solid is washed with ether (50 mL), the washings and the filtrate are combined, and the resulting solution is concentrated with a rotary evaporator (about 60 Torr, about 30 ° C.). The concentrate is filtered and the solid is washed with ether (10 mL). The washings and the filtrate are combined, and the resulting solution is concentrated with a rotary evaporator (about 60 Torr, about 30° C.). The resultant ligand, CH3OSi(CH3)2(CH2)3N(CH3)(CH2)2N(CH3)2, having the form of a light yellow liquid, is weighed (8.46 g, 36.4 mmol, 61%).

1. concentrationconcentrated with a rotary evaporator (about 10 Torr, about 45 ° C.)
2. additionThe concentrate is diluted with ether (50 mL)
3. filtrationfiltered
4. washThe solid is washed with ether (50 mL)
5. concentrationthe resulting solution is concentrated with a rotary evaporator (about 60 Torr, about 30 ° C.)
6. filtrationThe concentrate is filtered
7. washthe solid is washed with ether (10 mL)
8. concentrationthe resulting solution is concentrated with a rotary evaporator (about 60 Torr, about 30° C.)

ORD record

ord-c528ce21dfbe4aa8975639a6899d4754

Source dataset

uspto-grants-2003_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06593286B1