2-cyano-N-prop-2-ynylacetamide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 50 ml reaction flask equipped with a water separator and a reflux condenser was charged with 2.2 g of 2,3-dihydro-5,6-dimethoxy-3,3-dimethyl-1H-inden-1-one (see Example 1), 1.2 g of 2-cyano-N-prop-2-ynyl-acetamide (see above), catalytic amounts of pyrrolidine, and benzoic acid in 20 ml of toluene. The reaction mixture was refluxed for 24 hours with simultaneous separation of water. Then, the product in the cold reaction mixture was filtered off and recrystallized in ethylacetate to yield 1.13 g of white crystals, m.p. 202° C.-205° C. UV 362 nm (ε=24′992). Solubility: 0.04% in CÉTIOL LC A 50 ml reaction flask Then, the product in the cold reaction mixture was filtered off recrystallized in ethylacetate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 15.4 ml (240 mmol) of propargyl amine and 17.1 ml (160 mmol) of ethyl cyano acetate was heated for 7 hours to 40° C. in a reaction flask. The crystalline material formed was heated for another 17 hours to 70° C. Then, the cooled reddish product was dried at high vacuum to yield 18.4 g (94%) of a red powder, m.p. 100-103° C. was heated for 7 hours to 40° C. in a reaction flask The crystalline material formed was heated for another 17 hours to 70° C Then, the cooled reddish product was dried at high vacuum

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 15.4 ml (240 mmol) of propargyl amine and 17.1 ml (160 mmol) of ethyl cyano acetate was heated for 7 hours to 40° C. in a reaction flask. The crystalline material formed was heated for another 17 hours to 70° C. Then, the cooled reddish product was dried at high vacuum to yield 18.4 g (94%) of a red powder, m.p. 100-103° C. was heated for 7 hours to 40° C. in a reaction flask The crystalline material formed was heated for another 17 hours to 70° C Then, the cooled reddish product was dried at high vacuum

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 15.4 ml (240 mmol) of propargyl amine and 17.1 ml (160 mmol) of ethyl cyano acetate was heated for 7 hours to 40° C. in a reaction flask. The crystalline material formed was heated for another 17 hours to 70° C. Then, the cooled reddish product was dried at high vacuum to yield 18.4 g (94%) of a red powder, m.p. 100-103° C. was heated for 7 hours to 40° C. in a reaction flask The crystalline material formed was heated for another 17 hours to 70° C Then, the cooled reddish product was dried at high vacuum