Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-Mercaptoethanol → 2-[(3,6-Dichloro-4-pyridazinyl)thio]ethanol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-Mercaptoethanol | HCID 1567 | — |
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | 3,4,6-Trichloropyridazine | HCID 95123 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 2-[(3,6-Dichloro-4-pyridazinyl)thio]ethanol | HCID 81766083 | — |
반응 단계
A solution of 3,4,6-trichioropyridazine (25 g) in tetrahydrofuran (200 ml) and triethylamine (19 ml) was treated at 0° C. (ice bath cooling) with 2-mercaptoethanol (8.33 ml) over 5 minutes. After the addition was complete, the mixture was stirred at room temperature for 72 hours. The mixture was stirred with aqueous sodium bicarbonate solution and dichloromethane and the solid was collected, washed with water, ether and pentane and dried in vacuo, giving (22.9 g). The combined aqueous and organic fraction was evaporated to half volume giving further solid, which was washed and dried as above (5.0 g). The total yield of solid (27.9 g; 91%) contained some bromo-analogue (5-10%) by NMR.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07732460B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-ac95521bbf7746a397c2d885666fc1aa |
| 출처 메모 | uspto-grants-2010_06 |