反応 #1869179

反応方程式

hydrochloric acid

compound

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

potassium carbonate

t-butyl dicarbonate

→

title compound

収率 89.0%

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

収率 89.0%

溶媒

water

反応条件

後処理

1. 1
   抽出The aqueous layer was extracted three times with ethyl acetate
2. 2
   洗浄The combined organic layer was washed with a saturated aqueous solution of sodium chloride
3. 3
   乾燥dried over an anhydrous magnesium sulfate
4. 4
   濃縮concentrated
5. 5
   その他The residue was purified by column chromatography on silica gel (n-hexane:ethyl acetate=5:1→1:2)

実験手順

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.

出典