참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Benzoic acid, 2-amino-5-iodo- | HCID 72911 | — |
| 반응물 | 1,3-Bis(diphenylphosphino)propane | HCID 81219 | — |
| 반응물 | HCID 178418416 | HCID 178418416 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Amino-5-(methoxycarbonyl)benzoic acid | HCID 13105036 | — |
반응 단계
After dissolving 2-amino-5-iodobenzoic acid (4 mmol, 1052 mg) in DMF (10 ml) and MeOH (5 ml), NEt3 (3 eq, 1.67 ml) was added. Next, palladium acetate (0.1 eq, 90 mg) and dppp (0.1 eq, 165 mg) were added, carbon monoxide substitution was carried out, and the mixture was stirred at 80° C. for 5 hours. Upon completion of the reaction, acetic acid (2.5 ml) was added to suspend the reaction. Water (50 ml) was added, and extraction was performed with ethyl acetate (50 ml×3 times). The organic layer was washed with water (100 ml×2 times) and then dried over sodium sulfate. After concentration, a developing solvent (Hex/AcOEt=4/1→1/1) was used for purification by silica gel chromatography to obtain 2-amino-5-(methoxycarbonyl)benzoic acid. The compound was identified by LC-MS.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07517875B2 |
|---|
| 출처 데이터셋 | uspto-grants-2009_04 |
|---|
| ORD ID | ord-048688c5d3694dddb090ba85c4bb8d4f |
|---|
| 출처 메모 | uspto-grants-2009_04 |
|---|