HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86710463, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Caprolactam | HCID 7768 | — |
| Reactant | 2-Chlorobenzyl chloroformate | HCID 4072342 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 86710463 | HCID 86710463 | — |
Reaction Steps
1 g (8.8 mmol) of ε-caprolactam was dissolved in 3.88 g of 20 wt % NaOH solution and heated to reflux for 3-5 hours. After ε-caprolactam was hydrolyzed completely, the mixture was cooled down to 5˜10° C. and 5 g of water was added. 1.8 g (8.8 mmol) of 2-chlorobenzyl chloroformate was added dropwise. The mixture was stirred at room temperature for an hour and washed with 15 g of ethyl acetate twice. The pH of the aqueous layer was adjusted to 1-2 by adding 16% HCl and extracted with ethyl acetate twice. Combined ethyl acetate layer was washed with brine. The organic layer was dried by sodium sulfate and concentrated to obtain 6-(2-Chloro-benzyloxycarbonylamino)-hexanoic acid. Purity was 98.9%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08809581B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-c03a6ea23e0741a3905f9c822f2d2676 |
| Source note | uspto-grants-2014_08 |