Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Thiomorpholine → 4-[[(4-Thiomorpholinyl)methylene]amino]-3-pyridinol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Thiomorpholine | HCID 67164 | — |
| 반응물 | 4-[[(Dimethylamino)methylene]amino]-3-pyridinol | HCID 15380929 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 4-[[(4-Thiomorpholinyl)methylene]amino]-3-pyridinol | HCID 15380938 | — |
반응 단계
A mixture prepared from 4-[[(dimethylamino)methylene]amino]-3-pyridinol (5.14 g), thiomorpholine (10.5 ml, distilled from CaH2) and dry toluene (120 ml) was refluxed overnight. The reaction mixture was concentrated, triturated with diethyl ether, adhered to silica (methanol), flash chromatographed (10% methanol/ethyl acetate), and triturated with diethyl ether to yield 6.06 g of product. A 3.5 g sample was recrystallized from methanol, and dried under high vacuum and refluxing isopropanol to yield 2.13 g of crystals, m.p. 197°-198.5° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05869480 |
| 출처 데이터셋 | uspto-grants-1999_02 |
| ORD ID | ord-291c42efa7ff47deaf37615e4e62ac96 |
| 출처 메모 | uspto-grants-1999_02 |