반응 #1130

반응 방정식

pyridine

5-(trimethylsilyl)-3-(1-methyl-2-pyrrolidinyl)pyridine

fumaric acid

→

5-trimethylsilyl-3-(1-methyl-2-pyrrolidinyl)pyridine fumarate

수율 51.0%

용매

methanol

반응 조건

후처리

1. 1
   기타After 30 minutes the solvent was removed in vacuo
2. 2
   기타Trituration with diethyl ether followed by recrystallization from ethyl acetate

실험 절차

The above-described pyridine derivative was converted into invention compound of Formula I by the addition of one equivalent of fumaric acid to a methanol (5 mL) solution of the free amine at 25° C. After 30 minutes the solvent was removed in vacuo and the residue pumped under high vacuum. Trituration with diethyl ether followed by recrystallization from ethyl acetate afforded 5-trimethylsilyl-3-(1-methyl-2-pyrrolidinyl)pyridine fumarate, (51%). M.p. 161°-162° C. (EtOAc); 1H NMR (D2O, 300 MHz): δ 8.48 (s, 2 H), 8.26 (s, 1 H), 6.25 (s, 3 H), 4.24 (bm, 1 H), 3.53 (bm, 1 H), 3.03 (bm, 1 H), 2.43 (s, 3 H), 2.27 (m, 1 H), 1.9-2.1 (m, 3 H), 0.0 (s, 9 H).

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