HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → (1-Cyanocyclopropyl)methyl methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 1-(Hydroxymethyl)cyclopropane-1-carbonitrile | HCID 22028207 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | (1-Cyanocyclopropyl)methyl methanesulfonate | HCID 54220629 | 88.5% |
Reaction Steps
A stirred mixture of 1-(hydroxymethyl)cyclopropanecarbonitrile (24.30 mmol, 2.36 g) in dichloromethane (30 mL) was treated with triethylamine (48.6 mmol, 6.83 mL, 4.92 g) and portionwise with methanesulfonyl chloride (31.6 mmol, 2.445 mL, 3.62 g) keeping the reaction mixture at 0° C. The solution was allowed to stir for 1 hour then diluted with saturated sodium hydrogencarbonate and extracted with 10% methanol/dichloromethane (×3). The organic layers were combined and concentrated under reduced pressure to give the intermediate (1-cyanocyclopropyl)methyl methanesulfonate (3.77 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08759352B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-f1aee2912b6e42ba8fdfd6fadca482cb |
| Source note | uspto-grants-2014_06 |