HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 135456012, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 135494392 | HCID 135494392 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 135456012 | HCID 135456012 | — |
Reaction Steps
0.17 ml (2.17 mmoles) of methanesulfonyl chloride is added at 0° C. to 740 mg (1.81 mmoles) of the compound from Example 17 and 0.3 ml (2.17 mmoles) of triethylamine in 18 ml of absolute CH2Cl2. The mixture is allowed to come to room temperature and is stirred 30 minutes longer. The mixture is first extracted twice with 30 ml portions of 1 N NaOH and twice with 30-ml portions of 1 N HCl, the organic phase is dried over MgSO4, and the solvent is evaporated under vacuum in a rotary evaporator. The solid residue is stirred with a mixture of 30 ml ethyl acetate and 30 ml petroleum ether, and the product is filtered off. Yield: 650 mg (73.8%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06187779B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-914228035c9e4977a4536bdbe0a7e23a |
| Source note | uspto-grants-2001_02 |