Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dibromomethane → 4-(2-(5-bromo-4-(2-chloro-4-cyclopropyl-6-methylphenyl)-4H-1,2,4-triazol-3-ylthio)acetamido)-3-chlorobenzoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dibromomethane | HCID 3024 | — |
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Dichloroacetic Acid | HCID 6597 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 반응물 | 4-(2-(5-amino-4-(2-chloro-4-cyclopropyl-6-methylphenyl)-4H-1,2,4-triazol-3-ylthio)acetamido)-3-chlorobenzoic acid | HCID 59813099 | — |
| 촉매 | Benzyltriethylammonium bromide | HCID 165294 | — |
| 생성물 | 4-(2-(5-bromo-4-(2-chloro-4-cyclopropyl-6-methylphenyl)-4H-1,2,4-triazol-3-ylthio)acetamido)-3-chlorobenzoic acid | HCID 16221815 | 42% |
반응 단계
Dichloroacetic acid (0.065 mL, 0.78 mmol) was added to a mixture of compound 6 (192 mg, 0.39 mmol), benzyltriethyl ammonium bromide (318 mg, 1.17 mmol) and sodium nitrite (538 mg, 7.8 mmol) in dibromomethane (10 mL). The mixture was stirred at room temperature for 18 hours in the dark. The reaction mixture was then concentrated and the resulting residue was purified by prep. TLC (95% dichloromethane/5% methanol) to afford 88 mg, 42% yield of 4-(2-(5-bromo-4-(2-chloro-4-cyclopropyl-6-methylphenyl)-4H-1,2,4-triazol-3-ylthio)acetamido)-3-chlorobenzoic acid (7).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08252828B2 |
| 출처 데이터셋 | uspto-grants-2012_08 |
| ORD ID | ord-8f5442b5fc924f86808779fe20c60690 |
| 출처 메모 | uspto-grants-2012_08 |