HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 178418975, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 178418329 | HCID 178418329 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 178418975 | HCID 178418975 | — |
Reaction Steps
A solution of Intermediate 35 (90.3 g) in pyridine (415 ml) was added dropwise with methanesulfonyl chloride (42.4 ml) with stirring and ice cooling over 15 minutes and stirred with ice cooling for 30 minutes and at room temperature for 20 minutes. The reaction mixture was added with methanol (54.2 ml) to terminate the reaction, stirred at room temperature for 2.5 hours, further added with water (540 ml) and stirred at room temperature for 1 hour and with ice cooling for 1 hour. The deposited precipitates were collected by filtration, washed with water and then dried at 40° C. under reduced pressure to obtain the title compound (105 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07094789B2 |
| Source dataset | uspto-grants-2006_08 |
| ORD ID | ord-d2ae7ccd3f25492baf70cc5fa51d6131 |
| Source note | uspto-grants-2006_08 |