反応 #1552085

反応方程式

5-hydroxy-1-trimethylsilanyl-3,3a,4,5-tetrahydro-2H-cyclopenta[c]acridin-2-one

SOCl2

NaHCO3

→

5-Chloro-1-trimethylsilanyl-3,3a,4,5-tetrahydro-2H-cyclopenta[c]acridin-2-one

溶媒

DCM

反応条件

後処理

1. 1
   抽出the aqueous phase is extracted with DCM
2. 2
   洗浄the resulting organic phase is rinsed with a saturated aqueous solution of NaCl
3. 3
   乾燥dried over Na2SO4
4. 4
   ろ過filtered
5. 5
   その他evaporated
6. 6
   その他The residue obtained
7. 7
   その他is purified by flash chromatography

実験手順

The 5-hydroxy-1-trimethylsilanyl-3,3a,4,5-tetrahydro-2H-cyclopenta[c]acridin-2-one (323 mg, 1.00 mmol) is dissolved in 10 ml of freshly distilled DCM under an argon atmosphere at 0° C. SOCl2 (182 μl, 2.5 mmol) is then added dropwise to the reaction medium, which is stirred at 0° C. for 15 min. The reaction medium is then run into a saturated aqueous solution of NaHCO3, the aqueous phase is extracted with DCM and the resulting organic phase is rinsed with a saturated aqueous solution of NaCl, dried over Na2SO4, filtered and evaporated. The residue obtained is purified by flash chromatography.

出典