HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 18625053, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 1,4-Bis(2-hydroxyhexafluoroisopropyl)benzene | HCID 631065 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18625053 | HCID 18625053 | 56.5% |
Reaction Steps
4.1 g (10 mmol) of 1,4-bis-(2,2,2-trifluoro-1-hydroxy-1-trifluoromethylethyl)-benzene were dissolved in 50 ml of methylene chloride, and 2.5 g (25 mmol) of triethylamine were added. 2.86 g (25 mmol) of methanesulfonyl chloride were added dropwise at 5° to 10° C. The mixture was stirred for 48 hours at room temperature, separated off from the precipitated salt, washed with water, dried and evaporated down. The residue was chromatographed over a silica gel column with methylene chloride/n-hexane (1:1). 3.2 g of 1,4-bis-(2,2,2-trifluoro-1-methanesulfonyloxy-1-trifluoromethylethyl)-benzene were obtained (colorless crystals, m.p.: 151° C. [from diisopropyl ether]).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05716756 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-cb5d43291b3a4b9ba14c01ce9d49dd6f |
| Source note | uspto-grants-1998_02 |