Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) → HCID 25181625, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 반응물 | (1S,3R)-3-aminocyclohexanol | HCID 25630532 | — |
| 반응물 | 4-Chloro-5-(4-chlorophenyl)isoxazole-3-carboxylic acid | HCID 67121133 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 25181625 | HCID 25181625 | — |
반응 단계
To 18 mg (0.07 mmol) of 4-chloro-5-(4-chlorophenyl)isoxazole-3-carboxylic acid in anhydrous N,N-dimethylformamide (1 mL) was added O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (HATU; 27 mg, 0.07 mmol), followed by (1S,3R)-3-aminocyclohexanol (8.1 mg, 0.07 mmol) with stirring at room temperature. After 18 h, the solvent was removed in vacuo, and the residue was partitioned between water and ethyl acetate. The aqueous layer was separated and repeatedly extracted with ethyl acetate, the combined organic extracts were dried (MgSO4), the solvent removed in vacuo and the residue was purified by preparative HPLC to afford the title compound: (5.3 mg, 0.015 mmol). MS (ESI) m/z (M+H+): 354.9/356.9.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08211927B2 |
| 출처 데이터셋 | uspto-grants-2012_07 |
| ORD ID | ord-cf5e3ebce42044799c40d8ef36190588 |
| 출처 메모 | uspto-grants-2012_07 |