Water → HCID 86752907, compound

Participants

Reaction Steps

1.0 g (3.091 mmol) of dibenz[b,f]oxepin-10-ylmethyl-carbamic acid tert-butyl ester is placed in 10 ml of dimethylformamide, 0.22 g (4.636 mmol) of 55% sodium hydride suspension (in oil) is added at room temperature, the mixture is stirred for 15 minutes and then 0.279 ml (3.709 mmol) of propargyl bromide is added dropwise at room temperature. After 1 hour, water and a small amount of brine are carefully added and tert-butyl methyl ether is mixed in. The organic phase is washed 4× with water, dried over sodium sulfate and concentrated. 1.106 g (3.06 mmol)=98.8% of dibenz[b,f]oxepin-10-ylmethyl-prop-2-ynyl-carbamic acid tert-butyl ester are obtained in the form of a brown oil. TLC (silica gel, ethyl acetate/hexane=9:1; UV): Rf =0.45.

Provenance & Evidence