HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiophenol → HCID 3249365, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiophenol | HCID 7969 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Chloroethyl chloroformate | HCID 521305 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 3249365 | HCID 3249365 | 98.5% |
Reaction Steps
A solution of benzenethiol (50 g, 450 mmol) and 1-chloroethyl chloroformate (65 g, 450 mmol) in CH2Cl2 (300 mL) was cooled to 0-4° C. in an ice-water bath. To the mixture was added a solution of triethylamine (450 mmol) in dichloromethane (200 mL) dropwise over 30 min. The reaction was removed from the ice bath and stirred at ambient temperature for 12 h. The reaction was washed with water (3×500 mL), the organic phase was separated, dried over anhydrous magnesium sulfate and concentrated in vacuo to afford the product as a pale yellow liquid (96 g, 98.5%). 1H NMR (CDCl3, 400 MHz): δ 1.82 (d, 3H), 6.6 (q, 1H), 7.2-7.4 (m, 5H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08378137B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-0b6b5ae3d8e941868e520da55b697227 |
| Source note | uspto-grants-2013_02 |