반응 #78251

반응 방정식

chloromethyltrimethylsilane

2-(4-chlorophenyl)ethylamine

K2CO3

→

compound

수율 49.9%

4-Chloro-N-[(trimethylsilyl)methyl]benzeneethanamine

수율 49.9%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도The reaction mixture was refluxed for 13 h
2. 2
   온도after cooling
3. 3
   여과the precipitate was filtered off
4. 4
   농축the filtrate concentrated under vacuum
5. 5
   기타The resulting oil was chromatographed over silica gel (CH2Cl2/MeOH/Et3N: 97/2/1)

실험 절차

The compound of formula (P11), wherein n=2 and R″ is chloro, was prepared from a mixture of chloromethyltrimethylsilane (3.7 mL, 42.8 mmol), 2-(4-chlorophenyl)ethylamine (10 g, 64.25 mmol), and K2CO3 (4 g, 28.9 mmol) in acetonitrile (80 mL). The reaction mixture was refluxed for 13 h and after cooling, the precipitate was filtered off and the filtrate concentrated under vacuum. The resulting oil was chromatographed over silica gel (CH2Cl2/MeOH/Et3N: 97/2/1) to yield the above-referenced compound as a colorless oil (5.17 g). 1H NMR (CDCl3): 7.25 (2H, d, J=8.3 Hz), 7.12 (2H, d, J=8.3 Hz), 2.7-2.9 (4H, m), 2.08 (3H, s), 0.95 (1H, br s), 0.02 (9H, s).

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