HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13371578, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 13371559 | HCID 13371559 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 13371578 | HCID 13371578 | 127.2% |
Reaction Steps
400 mg of 6-piperidinocarbonyl-4-methyl-β-carboline-3-carboxylic acid ethyl ester is heated in 16 ml of toluene with 200 mg of Lawesson's reagent [2,4-bis(4-methoxyphenyl)-1,3-dithiaphosphetane-2,4-disulfide] for one hour to 100° C. Thereafter the mixture is combined with water and extracted twice with ethyl acetate. The ethyl acetate phase is dried, filtered, concentrated, and chromatographed over silica gel with methylene chloride/ethanol=10:1. Recrystallization of the corresponding fractions from ethanol/water yields 240 mg of 6-piperidinothiocarbonyl-4-methyl-β-carboline-3-carboxylic acid ethyl ester, mp 225°-230° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04600715 |
| Source dataset | uspto-grants-1986_07 |
| ORD ID | ord-0d070676648a43359873f0e636f852b3 |
| Source note | uspto-grants-1986_07 |