HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Rac-ethyl (1s,4s)-4-(methanesulfonyloxy)cyclohexane-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Ethyl 4-hydroxycyclohexanecarboxylate | HCID 86973 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Rac-ethyl (1s,4s)-4-(methanesulfonyloxy)cyclohexane-1-carboxylate | HCID 58812756 | — |
Reaction Steps
Methanesulfonyl chloride (2.4 mL, 31 mmol) was slowly added to a dichloromethane solution (75 mL) of ethyl 4-hydroxycyclohexanecarboxylate (4.63 mL, 28.7 mmol) and triethylamine (8.2 mL, 59 mmol) at 0° C. The reaction mixture was stirred for 30 minutes, concentrated in vacuo and diluted in diethyl ether (100 mL). The solution was washed with 10% hydrochloric acid (25 mL), water (25 mL), and saturated sodium bicarbonate (15 mL). The organics were dried (magnesium sulfate) and concentrated in vacuo to afford the title compound. 1H NMR (500 MHz, CDCl3) δ 1.23 (t, J=7.1 Hz, 3H), 1.54-1.82 (m, 4H), 1.87-1.97 (m, 2H), 2.00-2.08 (m, 2H), 2.34-2.41 (m, 1H), 3.00 (s, 3H), 4.13 (q, J=7.1 Hz, 2H), 4.88-4.92 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08053455B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-e18a53d7fc534d01b4ec1198b834a291 |
| Source note | uspto-grants-2011_11 |