Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
N,N-Dimethylaniline → 7-Chloro-5-[[(2,3-difluorophenyl)methyl]thio]-thiazolo[4,5-d]pyrimidin-2-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | N,N-Dimethylaniline | HCID 949 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 5-(2,3-Difluorobenzylthio)-2-aminothiazolo[4,5-d]pyrimidin-7-ol | HCID 135531169 | — |
| 생성물 | 7-Chloro-5-[[(2,3-difluorophenyl)methyl]thio]-thiazolo[4,5-d]pyrimidin-2-amine | HCID 11221650 | 31% |
반응 단계
The product of step (c) (10.0 g) was suspended in phosphoryl chloride (55 ml). N,N-dimethylaniline (5.5 ml) added slowly and reaction mixture heated at reflux for 2 hours. Allowed to cool, then poured on to ice with vigorous stirring; temperature was not allowed to go above 45° C. (ice added). After approximately 20 minutes the temperature stabilized at 30° C. The solid that formed was collected by filtration and washed with water. Purified by column chromatography (EtOAc to 5% MeOH in EtOAc) to give 3.34 g of product. 31% yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07585867B2 |
| 출처 데이터셋 | uspto-grants-2009_09 |
| ORD ID | ord-a78f9fbfce444e5b9302ca7f268ac233 |
| 출처 메모 | uspto-grants-2009_09 |