Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Fumaric Acid → 5-Trimethylsilyl-3-(1-methyl-2-pyrrolidinyl)pyridine fumarate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Fumaric Acid | HCID 444972 | — |
| 반응물 | 5-(Trimethylsilyl)-3-(1-methyl-2-pyrrolidinyl)pyridine | HCID 19694296 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 5-Trimethylsilyl-3-(1-methyl-2-pyrrolidinyl)pyridine fumarate | HCID 19694303 | 51% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05723477 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-c2497e75ae4e46b1beb5da566107c8e5 |
| 출처 메모 | uspto-grants-1998_03 |