HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86602386, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 58256115 | HCID 58256115 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86602386 | HCID 86602386 | — |
Reaction Steps
A solution of the product from step (e) (1.99 g, 8.25 mmol) in CH2Cl2 (41 ml) was cooled to 0° C. and treated with triethylamine (3.4 ml, 24.7 mmol) followed by dropwise addition of methanesulfonyl chloride (1.4 ml, 18.1 mmol) over 10 min. After 45 minutes, the crude reaction was diluted with CH2Cl2 (100 ml) and washed with ice water (25 ml), 10% citric acid (2×25 ml), sat. NaHCO3 (2×25 ml) and brine (1×25 ml). The organic layer was dried (MgSO4), concentrated to 20 ml and diluted with anhydrous dioxane (76 ml). This mixture was concentrated to remove remaining CH2Cl2 and the resulting dioxane solution was carried forward to the next reaction.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07893051B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-52c61234f38b414fa12dbeedd200bc1a |
| Source note | uspto-grants-2011_02 |