HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl trifluoromethanesulphonate → HCID 86750985, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl trifluoromethanesulphonate | HCID 67924 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 19041813 | HCID 19041813 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86750985 | HCID 86750985 | — |
Reaction Steps
2-[-N-acetyl[{2,6-dimethoxy-4-(3-(3,4,5-trimethoxyphenyl)-2,4-dithiolanyl)phenoxy}ethoxycarbonyl]aminomethyl]pyridine (32) (FIG. 26) (0.049 g, 0.076 mmole), diisopropylethylamine (8 μl, 0.076 mmole) and 5 ml anhydrous dichloromethane were cooled to 0° C. under a nitrogen atmosphere. Ethyl triflate (10 μl, 0.076 mmole) was added. The reaction was allowed to warm to room temperature and was stirred for 12 hours. The solvent was removed in vacuo and the remaining residue redissolved in 0.5 ml acetone. The acetone solution was purified by flash column chromatography using 100% ethyl acetate-10/1CHCl3MeOH-4/1CHCl3 /MeOH as eluent. The product was isolated as a 1.6/1.0 trans/cis mixture of diastereomers as a white foam (0.047 g. 75%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05639782 |
| Source dataset | uspto-grants-1997_06 |
| ORD ID | ord-e7e0e4c083214fe9b081b0dd61eef770 |
| Source note | uspto-grants-1997_06 |