반응 #218719

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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

수율 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

수율 58.9%

용매

DCM

DCM

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후처리

1. 1
   추출The mixture is extracted with DCM
2. 2
   세척the organic phase is washed with water, with a saturated NaCl solution
3. 3
   건조dried over Na2SO4
4. 4
   기타the solvent is evaporated under vacuum
5. 5
   기타The residue is chromatographed on silica gel
6. 6
   세척eluting with the toluene/AcOEt (95/5; v/v) mixture

실험 절차

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.

출처