Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-Chlorobenzoic Acid → HCID 10010234, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-Chlorobenzoic Acid | HCID 8374 | — |
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 반응물 | 5-n-butyl-2,4-dihydro-2-[5-(propionylamino)-2-(trifluoromethyl)phenyl]-4-[(2'-sulfamoylbiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one | HCID 10258037 | — |
| 생성물 | HCID 10010234 | HCID 10010234 | 50% |
반응 단계
Following the procedure of Example 51, 5-n-butyl-2,4-dihydro-2-[5-(propionylamino)-2-(trifluoromethyl)phenyl]-4-[(2'-sulfamoylbiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one (from Step F) was reacted with 2-chlorobenzoic acid (3 equivalents), CDI (3 equiv), and DBU (3 equiv). Flash chromatography of the crude product on silica gel (gradient elution with 0.5-2% MeOH in CH2Cl2) afforded a 50% yield of the title compound as a solid, mp 102°-105° C.; homogeneous by TLC in 9:1 CH2Cl2 --MeOH; mass spectrum (FAB) m/e 740 (M+1)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05411980 |
| 출처 데이터셋 | uspto-grants-1995_05 |
| ORD ID | ord-1df9d20720c94b3b98ac3118edd9fafa |
| 출처 메모 | uspto-grants-1995_05 |