Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → Tris(1,1-dimethylethyl) 2-{2-chloro-5-fluoro-6-[(3-thienylmethyl)amino]-4-pyrimidinyl}-1,1,2-hydrazinetricarboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Thiophenemethylamine | HCID 2776381 | — |
| 반응물 | Tris(1,1-dimethylethyl) 2-(2,6-dichloro-5-fluoro-4-pyrimidinyl)-1,1,2-hydrazinetricarboxylate | HCID 58000755 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Tris(1,1-dimethylethyl) 2-{2-chloro-5-fluoro-6-[(3-thienylmethyl)amino]-4-pyrimidinyl}-1,1,2-hydrazinetricarboxylate | HCID 86637009 | 99.1% |
반응 단계
Tris(1,1-dimethylethyl)2-(2,6-dichloro-5-fluoro-4-pyrimidinyl)-1,1,2-hydrazinetricarboxylate (1.413 g, 2.85 mmol) was dissolved in THF (5 mL). To this solution was added triethylamine (0.48 mL, 3.4438 mmol), followed by commercially available (3-thienylmethyl)amine (0.322 g, 2.85 mmol) which was dissolved in THF (1 mL). After stirring, the reaction mixture was diluted with water, and the aqueous layer was extracted with ethyl acetate. The organics were dried (Na2SO4) and concentrated to produce tris(1,1-dimethylethyl)2-{2-chloro-5-fluoro-6-[(3-thienylmethyl)amino]-4-pyrimidinyl}-1,1,2-hydrazinetricarboxylate as a white solid (1.6214 g, 99%). LCMS: (M+H−3Boc)+=374.1.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07893056B2 |
| 출처 데이터셋 | uspto-grants-2011_02 |
| ORD ID | ord-80beed6db33145ddb1d540651328e397 |
| 출처 메모 | uspto-grants-2011_02 |