HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 57901784, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 57901813 | HCID 57901813 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57901784 | HCID 57901784 | 71% |
Reaction Steps
To a solution of N-(2-bromoethyl)-7-[(2-thienylsulfonyl)amino]-1H-indole-2-carboxamide (0.35 g) in tetrahydrofuran (6 mL) was slowly added sodium hydride (60% in oil, 0.04 g) at 0° C., and the mixture was stirred at room temperature overnight. To the reaction mixture was added 10% aqueous citric acid solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4) and concentrated. The obtained residue was subjected to silica gel column chromatography and the title compound (0.20 g, yield 71%) was obtained as colorless crystals from a fraction eluted with ethyl acetate. The crystals were recrystallized from ethyl acetate-hexane. melting point>260° C. (decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957070B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-e0e131ed3de8455bbcd539a15f741e68 |
| Source note | uspto-grants-2015_02 |