Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 4-Oxo-4-{4'-[3-(propane-2-sulfonylamino)-thiophen-2-yl]-biphenyl-4-yl}-butyric acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 3-(4-Bromobenzoyl)propionic acid | HCID 80646 | — |
| 반응물 | Sodium Carbonate Monohydrate | HCID 2735133 | — |
| 반응물 | Propane-2-sulfonic acid {2-[4-(4,4,5,5-tetramethyl-[1,3,2] dioxaborolan-2-yl)-phenyl]-thiophen-3-yl}-amide | HCID 59747992 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | 4-Oxo-4-{4'-[3-(propane-2-sulfonylamino)-thiophen-2-yl]-biphenyl-4-yl}-butyric acid | HCID 69251351 | — |
반응 단계
Heat in a sealed tube with stirring propane-2-sulfonic acid{2-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-thiophen-3-yl}-amide (0.5 mmol), 4-(4-Bromo-phenyl)-4-oxo-butyric acid (0.75 mmol), 2M Na2CO3 water solution (0.2 mL) and Pd(PPh3)4 (0.05 mmol) in 4.0 ml of an anhydrous DME to 100° C. for 24 h. Evaporate and purify the filtrate by flash chromotography (Silica gel-hexane/EtOAc). Add NaOH 2M (1 ml) to a suspension of the resultant ester (0.128 mmol) in ethanol (1 ml) and stir 24 h. Add 6N HCl until pH is approximately 1 and a white solid precipitates. Filter the solid to provide the title compound. MS (ES−): 456 (M−1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07393868B2 |
| 출처 데이터셋 | uspto-grants-2008_07 |
| ORD ID | ord-225767fe43c844488612b31349ac800e |
| 출처 메모 | uspto-grants-2008_07 |