참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | Methyl 4-[2-(4-{[(2-amino-4,5,6,7-tetrahydro-1-benzothiophen-3-yl)carbonyl]amino}phenyl)ethyl]benzoate | HCID 68207883 | — |
| 반응물 | HCID 178464526 | HCID 178464526 | — |
| 촉매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 178464524 | HCID 178464524 | 70.8% |
반응 단계
A mixture of 319 mg of 3-{ethyl[trans-4-(methoxycarbonyl)cyclohexyl]sulfamoyl}benzoic acid, 0.10 mL of oxalyl chloride, 2.5 mL of dichloromethane, and one drop of DMF was stirred at room temperature for 2 hours, and then the reaction mixture was concentrated under reduced pressure. A mixture of the obtained crude product and 2.5 mL of dichloromethane was added to a mixture of 0.050 mL of pyridine, 250 mg of methyl 4-[2-(4-{[(2-amino-4,5,6,7-tetrahydro-1-benzothiophen-3-yl)carbonyl]amino}phenyl)ethyl]benzoate, and 2.5 mL of dichloromethane, followed by stirring at room temperature overnight. The reaction mixture was purified by silica gel column chromatography (hexane-chloroform) to obtain 320 mg of methyl 4-(2-{4-[({2-[(3-{ethyl[trans-4-(methoxycarbonyl)cyclohexyl]sulfamoyl}benzoyl)amino]-4,5,6,7-tetrahydro-1-benzothiophen-3-yl}carbonyl)amino]phenyl}ethyl)benzoate as a yellow foamed solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08729068B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_05 |
|---|
| ORD ID | ord-8e554f0c4cfd402e889ade31902d6bbb |
|---|
| 출처 메모 | uspto-grants-2014_05 |
|---|