HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 10144265, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 2,4,6-Triisopropylphenylacetic acid | HCID 10515641 | — |
| Reactant | HCID 54144007 | HCID 54144007 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 10144265 | HCID 10144265 | 69.1% |
Reaction Steps
Oxalyl chloride (0.6 mL, 6.9 mmol) was added dropwise to a solution of 2,4,6-triisopropylphenyl acetic acid (1.52 g, 5.8 mmol) in 150 mL toluene with 4 drops of N,N-dimethylformamide as a catalyst. The resulting solution was stirred overnight and then concentrated in vacuo. The residue was redissolved in 150 mL dichloromethane. Sulfamic acid 2,6-diisopropyl-4-thiocyanato-phenyl ester (1.70 g, 5.8 mmol) and triethylamine (2.0 mL) were added, and the resulting mixture was stirred for 2 hours. Washed with 1M HCl, dried the organic layer over magnesium sulfate, filtered, and concentrated to give 2.24 g of [(2,4,6-triisopropyl-phenyl)-acetyl]-sulfamic acid 2,6-diisopropyl-4-thiocyanato-phenyl ester as a white solid; mp 164-165° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06093744 |
| Source dataset | uspto-grants-2000_07 |
| ORD ID | ord-f06acbcbb1d3460c81374aedaece22a5 |
| Source note | uspto-grants-2000_07 |