HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 67486828, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 1-(Methylsulfonyl)piperazine | HCID 709161 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | HCID 86619906 | HCID 86619906 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 67486828 | HCID 67486828 | 79.2% |
Reaction Steps
A mixture of N-[2-(benzylthio)-3-oxopropyl]-7-[methyl(pyridin-2-ylsulfonyl)amino]-5-[3-(methylsulfonyl)propoxy]-1H-indole-2-carboxamide (0.35 g), N-methylsulfonylpiperazine (0.18 g) and 1,2-dichloroethane (8 mL) was stirred at room temperature for 20 min. Sodium triacetoxyborohydride (345 mg) was added to the reaction solution, and the mixture was stirred at room temperature for 16 hr. The reaction solution was acidified with aqueous citric acid solution, and basified with aqueous sodium hydrogencarbonate solution. The precipitated crystals were collected by filtration, washed with water and ethyl acetate, and dried to give the title compound (341 mg, yield: 43%) as colorless crystals. MS: 794 (MH+). melting point: 195-196° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652133B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-780c2b58d2b2478c90dde13c9ad56111 |
| Source note | uspto-grants-2010_01 |