Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylcarbamoyl Chloride → 4-[[(Diethylamino)methylene]amino]-3-pyridinol N,N-dimethyl carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | N,N-Diethyl-N'-(3-hydroxypyridin-4-yl)methanimidamide | HCID 15380930 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 4-[[(Diethylamino)methylene]amino]-3-pyridinol N,N-dimethyl carbamate | HCID 67749077 | 70.3% |
반응 단계
To a solution prepared from 4-[[(diethylamino)methylene]amino]-3-pyridinol (3.12 g), triethylamine (3.34 g) and tetrahydrofuran (50 mL) was added N,N-dimethylcarbamyl chloride (2.28 g) under nitrogen. The resulting mixture was stirred at ambient temperature for 6 hours, diluted with ether (50 mL) and filtered. The filtrate was concentrated under reduced pressure and the residue chromatographed on silica gel (elution with 10% methanol in dichloromethane) to give 3.00 g of solid. Recrystallization from ether/hexanes afforded 1.57 g of crystalline solid, m.p. 73°-74° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05821239 |
| 출처 데이터셋 | uspto-grants-1998_10 |
| ORD ID | ord-d499d14d330d400ba93eabe225f7d895 |
| 출처 메모 | uspto-grants-1998_10 |