HuagongsheHuagongshe Chemistry Print Report · For research reference only
Putrescine → HCID 15728468, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Putrescine | HCID 1045 | — |
| Reactant | 1-Bromo-3-chlorobenzene | HCID 7928 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Acetic acid, 2-chloro-2,2-difluoro-, ethyl ester | HCID 67843 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 15728468 | HCID 15728468 | 50% |
Reaction Steps
A solution of 25 g of 3-bromochlorobenzene in 100 ml ether was added to a solution of 15.1 g of tetramethylenediamine, 52.4 ml of a 2.5M solution of n-butyllithium in hexane and 75 ml ether at -78° C. under nitrogen. After 1 hour, a solution of 31.0 g of ethyl chlorodifluoroacetate in 150 ml ether was added. After warming to room temperature, the reaction was poured into excess ammonium chloride solution and extracted with ether. The extracts were dried (Na2SO4) and evaporated. The residue was distilled (0.1 mm Hg) to give 14.7 g of an oil which was used directly.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05006563 |
| Source dataset | uspto-grants-1991_04 |
| ORD ID | ord-c2a0cf05097449d686c746e56af25384 |
| Source note | uspto-grants-1991_04 |