반응 #74650

반응 방정식

Tert-butyl 3-hydrazinoazetidine-1-carboxylate

Acetic acid

(2E)-1-(5-chloro-2-hydroxyphenyl)-3-(dimethylamino)prop-2-en-1-one

→

title compound

Tert-butyl 3-[5-(5-chloro-2-hydroxyphenyl)-1H-pyrazol-1-yl]azetidine-1-carboxylate

용매

ethanol

반응 조건

후처리

1. 1
   온도to warm to room temperature
2. 2
   온도The resulting suspension was cooled to 0° C.
3. 3
   여과the solid was filtered off
4. 4
   세척washed with cold ethanol (2×40 mL)
5. 5
   기타dried

실험 절차

Tert-butyl 3-hydrazinoazetidine-1-carboxylate, (Preparation 696, 88.37 g, 0.4247 mol) was dissloved in ethanol (883.7 mL) and the solution was cooled to 0° C. in an ice bath. Acetic acid (97.36 mL, 1.70 mol) was added followed by (2E)-1-(5-chloro-2-hydroxyphenyl)-3-(dimethylamino)prop-2-en-1-one, (Preparation 852, 95.86 g, 0.4247 mol) and the resulting slurry was allowed to warm to room temperature then stirred at room temperature for 2 days. The resulting suspension was cooled to 0° C. and the solid was filtered off, washed with cold ethanol (2×40 mL) and dried to give the title compound as a white granular solid, (83.23 g).

출처