Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
p-Xylyl bromide → tert-Butyl 4-{2-[(4-methylbenzyl)sulfonyl]thieno[3,2-c]pyridin-4-yl}piperazine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | p-Xylyl bromide | HCID 7721 | — |
| 반응물 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 반응물 | Lithium 4-chlorothieno[3,2-c]pyridine-2-sulfinate | HCID 86591057 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | tert-Butyl 4-{2-[(4-methylbenzyl)sulfonyl]thieno[3,2-c]pyridin-4-yl}piperazine-1-carboxylate | HCID 67157698 | — |
반응 단계
Lithium 4-chlorothieno[3,2-c]pyridine-2-sulfinate (0.44 mmol) was treated with 4-methylbenzylbromide (0.59 mmol) as described in Method P above and then reacted further with tert-butyl-piperazine-1-carboxylate as described in Method Q. Yield 0.005 g (3% over two steps). Beige solid. 1H NMR (300 MHz, CDCl3) δ 8.15 (d, J=6 Hz 1H), 7.40 (s, 1H), 7.00-7.16 (m, 4H), 4.42 (s, 2H), 3.46-3.60 (m, 4H), 3.37-3.46 (m, 4H), 2.34 (s, 3H), 1.49 (s, 9H); MS (ESI+) for C24H29N3O4S2 m/z 488 (M+H)+. HPLC 69%, RT 2.06 min (YMC ODS AQ, 33×3 mm, 10-90% acetonitrile in 3 min).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07943639B2 |
| 출처 데이터셋 | uspto-grants-2011_05 |
| ORD ID | ord-84520229000d48ce8e1f14a832bee125 |
| 출처 메모 | uspto-grants-2011_05 |