반응 #2495305

반응 방정식

cyclopropanesulfonic acid [4,4-dimethyl-2-(3-morpholin-4-yl-phenyl)-1,2,3,4-tetrahydro-quinoline-6-carbonyl]-amide

potassium carbonate

→

cyclopropanesulfonic acid [4,4-dimethyl-2-(3-morpholin-4-yl-phenyl)-1,2,3,4-tetrahydro-quinoline-6-carbonyl]-methyl-amide

수율 19.7%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONwas added idomethane (0.02 mL, 0.32 mmol)
2. 2
   추출The reaction mixture was extracted with ethyl acetate (2×50 mL)
3. 3
   세척washed with water (2×20 mL)
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   농축concentrated in vacuo
6. 6
   기타Purification by Waters automated flash system (column: Xterra 30 mm×100 mm, sample manager 2767, pump 2525, detector: ZQ mass and UV 2487, solvent system: acetonitrile and 0.1% ammonium hydroxide in water)

실험 절차

To a mixture of cyclopropanesulfonic acid [4,4-dimethyl-2-(3-morpholin-4-yl-phenyl)-1,2,3,4-tetrahydro-quinoline-6-carbonyl]-amide (100 mg, 0.21 mmol), and potassium carbonate (89.4 mg, 0.64 mmol) in N,N-dimethylformamide (4 mL) was added idomethane (0.02 mL, 0.32 mmol). The reaction mixture was stirred at 25° C. for 3 h. The reaction mixture was extracted with ethyl acetate (2×50 mL), washed with water (2×20 mL), dried over anhydrous sodium sulfate and then concentrated in vacuo. Purification by Waters automated flash system (column: Xterra 30 mm×100 mm, sample manager 2767, pump 2525, detector: ZQ mass and UV 2487, solvent system: acetonitrile and 0.1% ammonium hydroxide in water) afforded cyclopropanesulfonic acid [4,4-dimethyl-2-(3-morpholin-4-yl-phenyl)-1,2,3,4-tetrahydro-quinoline-6-carbonyl]-methyl-amide (20 mg, 19%) as a white solid: MS (ESI) M+1=484.3.

출처