反応 #64891

反応方程式

crude product

4-(9,10-DIHYDRO-10-METHYL-9-ACRIDINYL)-1-(2,2,2-TRICHLOROETHYLOXYCARBONYL)PIPERIDINE

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title compound

9,10-DIHYDRO-10-METHYL-9-(4-PIPERIDINYL)ACRIDINE

溶媒

acetic acid

反応条件

後処理

1. 1
   ろ過The reaction mixture is filtered after 30 minutes
2. 2
   濃縮concentrated in vacuo
3. 3
   workup.ADDITIONThe residue is then diluted with water
4. 4
   抽出extracted with CH2Cl2
5. 5
   乾燥The extract is dried with Na2SO4
6. 6
   ろ過filtered
7. 7
   濃縮concentrated in vacuo
8. 8
   その他The residue is then purified via flash chromatography (MeOH/CH2Cl2)

実験手順

Zinc dust (1.3 g, 20 mmol) is added to a solution of the crude product from step A in 20 mL glacial acetic acid maintained at 85° C. The reaction mixture is filtered after 30 minutes and concentrated in vacuo. The residue is then diluted with water, basified with a 1.0N aqueous NaOH solution, and extracted with CH2Cl2. The extract is dried with Na2SO4, filtered and concentrated in vacuo. The residue is then purified via flash chromatography (MeOH/CH2Cl2) to provide the title compound.

出典