HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dibromomethane → 4-(2-(5-bromo-4-(7-methoxy-4-methylnaphthalen-1-yl)-4H-1,2,4-triazol-3-ylthio)acetamido)-3-chlorobenzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dibromomethane | HCID 3024 | — |
| Reactant | Dichloroacetic Acid | HCID 6597 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Reactant | 4-(2-(5-amino-4-(7-methoxy-4-methylnaphthalen-1-yl)-4H-1,2,4-triazol-3-ylthio)acetamido)-3-chlorobenzoic acid | HCID 59813114 | — |
| Catalyst | Benzyltriethylammonium bromide | HCID 165294 | — |
| Product | 4-(2-(5-bromo-4-(7-methoxy-4-methylnaphthalen-1-yl)-4H-1,2,4-triazol-3-ylthio)acetamido)-3-chlorobenzoic acid | HCID 16058697 | 24% |
Reaction Steps
Dichloroacetic acid (0.1 mL, 1.2 mmol) was added to a mixture of compound 10 (304 mg, 0.6 mmol), benzyltriethyl ammonium bromide (492 mg, 1.8 mmol) and sodium nitrite (828 mg, 12 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 column chromatography (95% dichloromethane/5% methanol) to afford 80 mg, 24% yield of 4-(2-(5-bromo-4-(7-methoxy-4-methylnaphthalen-1-yl)-4H-1,2,4-triazol-3-ylthio)acetamido)-3-chlorobenzoic acid (11).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08003681B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-917dedf0abbd4f23a3fc7b16247e4278 |
| Source note | uspto-grants-2011_08 |