반응 #428509

반응 방정식

DMF

Example 1

4-(5-bromothiazol-2-yl)-2-chlorobenzaldehyde

sodium bicarbonate

1-hydroxybenzotriazole

1-(dimethylaminopropyl)-3-ethylcarbodiimide

ammonia ethanol

→

title compound

1-(4-(5-(4-isopropoxyphenyl)thiazol-2-yl)benzyl)azetidine-3-carboxamide

용매

chloroform

반응 조건

후처리

1. 1
   기타to terminate
2. 2
   기타the reaction
3. 3
   추출After the aqueous layer was extracted with chloroform twice
4. 4
   세척the combined organic layer was washed with saturated brine
5. 5
   건조After the organic layer was dried over anhydrous magnesium sulfate
6. 6
   기타the solvent was evaporated under reduced pressure
7. 7
   기타The resulting residue was purified on column chromatography (MeOH:CHCl3=1:10)

실험 절차

The compound obtained in the Example 1 (150 mg) was suspended in DMF (30 ml), and 1-hydroxybenzotriazole (74.4 mg), 1-(dimethylaminopropyl)-3-ethylcarbodiimide (106 mg), and a 2 M-ammonia/ethanol solution (0.92 ml) was added to the suspension at room temperature. After the mixture was stirred overnight, chloroform and saturated sodium bicarbonate aqueous solution were added to terminate the reaction. After the aqueous layer was extracted with chloroform twice, the combined organic layer was washed with saturated brine. After the organic layer was dried over anhydrous magnesium sulfate, the solvent was evaporated under reduced pressure. The resulting residue was purified on column chromatography (MeOH:CHCl3=1:10) to obtain the title compound (128 mg) as a pale yellow solid.

출처