반응 #49129

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2-(methylthio)-4,6-bis(trifluoromethyl)benzoyl chloride

(+)-[2-methyl-1-phenyl-2-(1-pyrrolidinyl)propyl]amine

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title product

수율 85.0%

N-[2-Methyl-1-phenyl-2-(1-pyrrolidinyl)propyl]-2-(methylthio)-4,6-bis(trifluoromethyl)benzamide

수율 85.0%

용매

DCM

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후처리

1. 1
   기타The volatile components were removed under reduced pressure
2. 2
   기타the residue chromatographed on silica gel
3. 3
   세척Elution with 0-80% ethyl acetate in pentane

실험 절차

A solution of 2-(methylthio)-4,6-bis(trifluoromethyl)benzoyl chloride D55 (60 mg; 0.19 mmol) in dry DCM (1 ml) was treated with (+)-[2-methyl-1-phenyl-2-(1-pyrrolidinyl)propyl]amine D6 (60 mg, 0.27 mmol) followed by triethylamine (5drops) and left overnight at room temperature. The volatile components were removed under reduced pressure and the residue chromatographed on silica gel. Elution with 0-80% ethyl acetate in pentane gave the title product as an oil (80 mg, 85%). 1H NMR (CDCl3) δ: 0.94 (3H, s), 1.00 (3H, s), 1.69 (4H, overlapping m), 2.54 (3H, s), 2.62 (2H, m), 2.72 (2H, m), 4.78 (1H, s), 7.25-7.45 (6H, overlapping m), 7.68 (1H, s), 7.72 (1H, s). Mass Spectrum (Electrospray LC/MS): Found 505 (MH+) C24H26F6N2OS requires 504. Ret time 2.24 min.

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