Dichloromethane → HCID 12571421, compound

Participants

Reaction Steps

To a solution of 2-butanone (6.2 ml, 69 mmol) and morpholine (18.1 ml, 208 mmol) in n-pentane (400 ml) was added dropwise 1 M titanium tetrachloride solution in dichloromethane (38.1 ml, 38.1 mmol) at 0-5° C. The cooling bath was removed and the mixture was stirred for 20 h. The precipitate was removed by filtration and washed with two 100-ml portions of diethyl ether. The filtrate was concentrated in vacuo. The residue was distilled over a vigreux column in a Kugelrohr oven (1 mbar, 40-70° C.) to give the title compound (5.1 g, 52%) as colorless oil.

Provenance & Evidence