반응 #1869179

반응 방정식

hydrochloric acid

compound

1-butyl-1,3,8-triazaspiro[4.5]decane-2,4-dione

potassium carbonate

t-butyl dicarbonate

→

title compound

수율 89.0%

1-butyl-8-(t-butoxycarbonyl)-1,3,8-triazaspiro-[4.5]decane-2,4-dione

수율 89.0%

용매

water

반응 조건

후처리

1. 1
   추출The aqueous layer was extracted three times with ethyl acetate
2. 2
   세척The combined organic layer was washed with a saturated aqueous solution of sodium chloride
3. 3
   건조dried over an anhydrous magnesium sulfate
4. 4
   농축concentrated
5. 5
   기타The residue was purified by column chromatography on silica gel (n-hexane:ethyl acetate=5:1→1:2)

실험 절차

To a solution of the compound prepared in Example 5 (326 mg) in water (3 mL) were added potassium carbonate and t-butyl dicarbonate (348 mg) subsequently, and the mixture was stirred for 1 hour at room temperature. The reaction mixture was neutralized with 1N hydrochloric acid. The aqueous layer was extracted three times with ethyl acetate. The combined organic layer was washed with a saturated aqueous solution of sodium chloride, dried over an anhydrous magnesium sulfate and then concentrated. The residue was purified by column chromatography on silica gel (n-hexane:ethyl acetate=5:1→1:2) to give the title compound (419 mg) having the following physical data.

출처