反応 #693346

反応方程式

7-(tert-butoxycarbonyl)-2-hydroxy-7-azaspiro[3.5]nonane

methanesulfonyl chloride

→

title compound

収率 100.0%

7-(tert-Butoxycarbonyl)-2-methanesulfonyloxy-7-azaspiro[3.5]nonane

収率 100.0%

溶媒

tetrahydrofuran

triethylamine

反応条件

後処理

1. 1
   workup.ADDITIONwere added
2. 2
   ろ過The reaction mixture was filtered
3. 3
   濃縮the filtrate was concentrated under reduced pressure
4. 4
   workup.ADDITIONAfter adding water
5. 5
   抽出to the residue, extraction
6. 6
   洗浄The organic layer was washed with water
7. 7
   乾燥dried over anhydrous magnesium sulfate
8. 8
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

実験手順

After dissolving 106 mg of 7-(tert-butoxycarbonyl)-2-hydroxy-7-azaspiro[3.5]nonane in 10 ml of tetrahydrofuran, 0.04 ml of methanesulfonyl chloride and 0.07 ml of triethylamine were added and the mixture was stirred overnight at room temperature. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. After adding water to the residue, extraction was performed with ethyl acetate. The organic layer was washed with water and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (148 mg, 100% yield).

出典