تفاعل #218719

معادلة التفاعل

acid chloride

7-Chloro-1-(2,4-dichlorophenyl)-1,5-dihydroisothiochromeno[4,3-c]pyrazole-3-carboxylic acid chloride

8-azaspiro[4.5]dec-8-ylamine hydrochloride

triethylamine

→

expected compound

المردود 58.9%

N-(8-azaspiro[4.5]dec-8-yl)-7-chloro-1-(2,4-dichlorophenyl)-1,5-dihydroisothiochromeno-[4,3-c]pyrazole-3-carboxamide

المردود 58.9%

المذيبات

DCM

DCM

ظروف التفاعل

المعالجة

1. 1
   استخلاصThe mixture is extracted with DCM
2. 2
   غسيلthe organic phase is washed with water, with a saturated NaCl solution
3. 3
   تجفيفdried over Na2SO4
4. 4
   أخرىthe solvent is evaporated under vacuum
5. 5
   أخرىThe residue is chromatographed on silica gel
6. 6
   غسيلeluting with the toluene/AcOEt (95/5; v/v) mixture

الإجراء التجريبي

A solution of 0.28 g of 8-azaspiro[4.5]dec-8-ylamine hydrochloride and 0.41 ml of triethylamine in 15 ml of DCM is cooled to 0° C., 0.6 g of the acid chloride prepared in Example 1, step A, in 10 ml of DCM is added dropwise and the mixture is left for 4 hours, with stirring, at RT. The mixture is extracted with DCM, the organic phase is washed with water, with a saturated NaCl solution, dried over Na2SO4 and the solvent is evaporated under vacuum. The residue is chromatographed on silica gel, eluting with the toluene/AcOEt (95/5; v/v) mixture. 0.45 g of the expected compound is obtained in amorphous form.

المصدر