반응 #92037

반응 방정식

HCl

1

Ethyl 7,7-dimethyl-5-phenyl-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine-3-carboxylate

KOH

H2O

→

title compound

수율 83.1%

(−)-7,7-Dimethyl-5-phenyl-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine-3-carboxylic acid

수율 83.1%

용매

EtOH

반응 조건

후처리

1. 1
   추출extracted with AcOEt
2. 2
   세척The extract was washed with brine
3. 3
   건조dried over MgSO4
4. 4
   농축concentrated in vacuo

실험 절차

A mixture of 1 (0.73 g) obtained in Example 1009, KOH (0.41 g), H2O (20 ml) and EtOH (20 mL) was stirred at 90° C. for 12 h, acidified with 1N HCl, and extracted with AcOEt. The extract was washed with brine, dried over MgSO4, and concentrated in vacuo to give 0.55 g (83% yield) of the title compound as colorless prisms ([α]D20° C.=−85.33, in CHCl3, C=0.46). mp 205-206° C., 1H NMR (CDCl3, 300 MHz): 1.59 (3H, s), 1.66 (3H, s), 2.05-2.15 (2H, m), 4.64 (1H, dd, J=9.6, 5.4 Hz), 6.04 (1H, s), 7.30-7.41 (5H, m), 7.73 (1H, s).

출처