Propargyl bromide → HCID 12786188, compound

A 0.25 ml. portion of propargyl bromide is added to a stirred suspension of 0.73 g. of magnesium and 6 mg. of mercuric chloride in 7.5 ml. of ether. The reaction is initiated after a few minutes of vigorous stirring at room temperature. A mixture of 3 g. of 80% 1-fluoro-2-hexanone and 3.63 g. of propargyl bromide in 7.5 ml. of ether is added dropwise through a dropping funnel so that the reaction remains gently refluxing (25° C. to 32° C.). Cooling in a water bath is required. The reaction mixture is cooled in an ice bath, quenched with 8 ml. of cold saturated aqueous ammonium chloride, filtered through Celite and washed with ether. The mother liquor is evaporated to dryness giving a reddish oily residue, which is Kugelrohr-distilled at 45° C./-4 mm giving the product as a colorless liquid.

1. waitThe reaction is initiated after a few minutes
2. additionA mixture of 3 g
3. temperatureremains gently refluxing (25° C. to 32° C.)
4. temperatureCooling in a water bath
5. temperatureThe reaction mixture is cooled in an ice bath
6. customquenched with 8 ml
7. filtrationof cold saturated aqueous ammonium chloride, filtered through Celite
8. washwashed with ether
9. customThe mother liquor is evaporated to dryness
10. customgiving a reddish oily residue, which
11. distillationis Kugelrohr-distilled at 45° C./-4 mm

ORD record

ord-298a3c664238423eac50792d1613a0b0

Source dataset

uspto-grants-1981_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04254036