HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → tert-Butyl ethyl {1-[3-(trifluoromethyl)phenyl]ethane-1,2-diyl}biscarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | tert-butyl N-{2-amino-1-[3-(trifluoromethyl)phenyl]ethyl}carbamate | HCID 43094068 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | tert-Butyl ethyl {1-[3-(trifluoromethyl)phenyl]ethane-1,2-diyl}biscarbamate | HCID 59536750 | — |
Reaction Steps
A solution of 500 mg (1.64 mmol) of the compound from Example 101A and 321 μl (2.30 mmol) of triethylamine in 15 ml of dichloromethane was cooled to 0° C. and admixed with 189 μl (1.97 mmol) of ethyl chloroformate. The ice bath was removed and the mixture was stirred for a further 1 h. The volatile constituents were removed on a rotary evaporator and the residue was purified by preparative HPLC [Method 20]. The product fractions were combined and freed from the solvents on a rotary evaporator. The residue was dried in an HV. This gave 527 mg (85% of theory) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08202895B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-d218a10a4ddb4154846689ca4730f76a |
| Source note | uspto-grants-2012_06 |