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. The temperature of the resultant mixture was returned to room temperature, and the mixture was stirred overnight. The reaction mixture was diluted with chloroform, washed with water and saturated brine and then dried over sodium sulfate anhydrate, and the solvent was distilled away under reduced pressure. The resultant residue was purified by silica gel thin layer chromatography (chloroform:methanol=20:1) and powdered with methanol-water to give the title compound (150 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07576135B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-68cad706609546e4a0c8f289f46ab21d |
| Source note | uspto-grants-2009_08 |