HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 59676768, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methyl (chlorosulfonyl)acetate | HCID 11435213 | — |
| Reactant | HCID 67056761 | HCID 67056761 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59676768 | HCID 59676768 | 54.3% |
Reaction Steps
The compound (230 mg) obtained in Example 95 and triethylamine (0.10 ml) were dissolved in methylene chloride (6.9 ml), and the mixture was cooled with ice. Methoxycarbonylmethanesulfonyl chloride (Synthesis, p. 321, 1975) (105 mg) was added, and the resultant mixture was warmed to room temperature and stirred overnight. The reaction mixture was diluted with chloroform, washed with water and saturated aqueous solution of sodium chloride and then dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The resultant residue was purified by preparative thin-layer chromatography on silica gel (chloroform:methanol=20:1) and powdered with methanol-water to obtain the title compound (150 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07365205B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-f57b58ab133640c1b68496cd4ce11858 |
| Source note | uspto-grants-2008_04 |