HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 18694219, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Chlorobutyryl chloride | HCID 78370 | — |
| Reactant | Methyl 4'-amino-2'-methyl[1,1'-biphenyl]-4-carboxylate | HCID 21948355 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18694219 | HCID 18694219 | 41.1% |
Reaction Steps
Methyl 4'-amino-2'-methylbiphenyl-4-carboxylate (D27) (1.84 g, 7.6 mmol) and triethylamine (2.6 ml, 19 mmol) were stirred in dichloromethane (100 ml) as 4-chlorobutyryl chloride (0.94 ml, 8.4 mmol) was added dropwise. The mixture was stirred for 1 h, vigorously stirred with water for 15 min, acidified (5M HCl), and separated. The organic phase was washed with water and K2CO3 /brine solution, dried (Na2SO4) and evaporated to give a light yellow solid. Chromatography on silica gel, eluting with 0-40% ether/dichloromethane, gave the title compound (1.08 g, 41%) as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05972935 |
| Source dataset | uspto-grants-1999_10 |
| ORD ID | ord-b6bbaa5c3ee3451babd34f2069ea6fe6 |
| Source note | uspto-grants-1999_10 |