反应详情

温度

100 °C

4.21 g of 1-(4-ethoxy-2,6-difluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]-pyrazole-3-carboximidamide 1-2-1 (13.2 mmol, 1.00 eq.) were suspended in 47 mL of dry 3-methyl-1 butanole, 0.26 mL of piperidine (2.63 mmol, 0.20 eq.) and 3.09 g of 3,3-bis(dimethylamino)-2-methoxypropanenitrile 1-3-1 (18.0 mmol, 1.37 eq.) were added under nitrogen atmosphere and stirred over night at 100° C. bath temperature. The reaction mixture was cold with an ice bath the precipitate was filtered of, washed with 3-methyl-1 butanol and dried at 50° C. to give 1.77 g (4.41 mmol, 33.5%) of analytically pure target compound.

1. additionwere added under nitrogen atmosphere
2. customThe reaction mixture was cold with an ice bath
3. filtrationthe precipitate was filtered of,
4. washwashed with 3-methyl-1 butanol
5. customdried at 50° C.
6. customto give 1.77 g (4.41 mmol, 33.5%) of analytically pure target compound